Size Distribution Measurements Research Articles

Extraction of E171 or E172 food additives from sugar-based or lipid-based complex matrices for primary particles identification by electron microscopy

Measurement of primary particle size distributions is fundamental to determining if a material should be classified as a nanomaterial according to the European Commission recommended definition. This is of particular relevance to alimentary products, where current regulation requires that any additives containing nanoforms be explicitly declared as such in the ingredients’ list. Currently, Electron Microscopy is the only instrumental technique able to reliably classify materials as nanomaterials. To verify the nanostatus of a material using this technique, it is essential to firstly extract the additives from the matrix in which they are dispersed, and then measure a wide size distribution while avoiding artefacts from the food matrix. In this operating procedure, extraction protocols, developed and applied for sugar-based or lipid-based food, are described. In particular, case studies for titanium dioxide E171 and iron oxide/iron hydroxide based materials such as E172 are considered. The protocols are based on gentle extraction of the additive materials and could, in principle, be used for other nanomaterials provided they are not soluble in water or ethanol and are resistant to enzymatic reactions. The size distribution of the extracted material can then be determined from images acquired using scanning and/or transmission electron microscopy.

The effect of different water types commonly applied during laser diffraction measurement on the particle size distribution of soils

It is expected in the future that soil particle size distribution (PSD) measurements by laser diffraction method (LDM) may replace sieve-pipette sedimentation methods (SPM) as they are faster, require less sample, and are accurate and reproducible. LDM measurement result is a continuous function of PSD, which can facilitate the conversion between the various limits (by countries, by scientific field) of the calculated particle size fractions (PSF – e.g. clay, silt, sand). Currently, there is no standard method for LDM PSD measurement. Many different types of instruments and preparation devices are currently used in laboratories, with various sample preparation, pre-treatment and measurement methods (duration, chemical and/or mechanical dispersion, settings, etc.). In soil LDM PSD measurements, researchers put relatively little emphasis on the choice of the type of aqueous media used. Thus, it is still questionable to what extent the results of the LDM measurement depend on the selection of the dispersion method and the aqueous media. For our research, eight soil samples with various physical and chemical properties were collected in Hungary. The particle size fractions (clay, silt, sand) determined with LDM (Malvern Mastersizer 3000) measured in three types of aqueous media (distilled, deionized and tap water), in different combinations of two dispersion methods (no treatment, ultrasonic or chemical dispersion with Calgon and their combination) were compared. For the comparison, PSF results of the conventional sieve pipette method (SPM) were used as a reference. Our results showed that LDM measurement can achieve various degrees of dispersion with different preparations, in many cases only partial dispersion, disaggregation, sometimes re-aggregation, and flocculation of soil particles were observed as compared to full preparation (in SPM). The “disaggregation pattern” of the soil samples also depended on the quality of the aqueous media and the properties of the soil investigated, because several types and degrees of interactions could occur in the various soil-liquid-dispersant/disaggregation effect systems.

The Árpád Mound – Geoarcheological Research of a Burial Mound in the Central Carpathian Basin

Kurgans hold exceptional archaeological, natural, and environmental historical significance in the lowland landscape of Eastern Europe, which has been extensively altered by millennia of agricultural activity. By conducting comparative soil and sedimentological analyses of the buried soil levels from kurgan construction, as well as the recent surface soil, we can uncover environmental changes from the latter half of the Holocene. These analyses also reveal how prehistoric human activities influenced local soil and environmental conditions. Our research focused on a geoarchaeological examination of a burial mound in the Hungarian Great Plain. Sedimentological analyses, including grain size distribution and magnetic susceptibility measurements, were performed on samples extracted by drilling from this mound. This comprehensive investigation enabled us to distinguish between different construction layers in the kurgan’s soil material and compare them. Additionally, it was possible to reconstruct steppe-like environmental conditions in the local surroundings of the kurgan before and during its construction.

Enhancing the performance and revealing the thermal behavior of the water-based coating derived from waterborne alkyd resins and totally methyl etherified amino resins

In this study, the curing parameters of the water-based coating were carefully optimized using waterborne alkyd resins as the matrix resin and totally methyl etherified amino resins as the crosslinking agent. Through an orthogonal experimental design and a controlled experiment, the optimal conditions, which were a 7:1 ratio of alkyd resins to amino resins and curing at 403.15 K for 30 min, were determined. Droplet size distribution and zeta potential measurements confirmed that the composite resin emulsion prepared with the optimal ratio was more uniformly and stably dispersed in water, which helped to optimize the coating and make it have excellent physical properties, mechanical stability and chemical durability. Thermal stability was also thoroughly evaluated by TGA analysis, paying particular attention to the third degradation stage of the optimized composite resin coating (573.15–733.15 K), pyrolysis kinetic analysis provided deeper insights into its thermal behavior. Activation energies calculated through both the KSA and Starink methods exhibited consistent values of 195.47 kJ/mol and 196.06 kJ/mol, respectively. Furthermore, a reaction mechanism function of G(α) = [−ln(1-α)]3 via C-R method implying a sigmoidal rate equation or stochastic nucleation. The activation energy calculated by this method is 211.10 kJ/mol and the pre-exponential factor is 2.22 × 1016 min−1. Notably, the thermodynamic parameters obtained from all three methods show remarkable agreement.

A scale-invariant log-normal droplet size distribution below the critical concentration for protein phase separation

Many proteins have been recently shown to undergo a process of phase separation that leads to the formation of biomolecular condensates. Intriguingly, it has been observed that some of these proteins form dense droplets of sizeable dimensions already below the critical concentration, which is the concentration at which phase separation occurs. To understand this phenomenon, which is not readily compatible with classical nucleation theory, we investigated the properties of the droplet size distributions as a function of protein concentration. We found that these distributions can be described by a scale-invariant log-normal function with an average that increases progressively as the concentration approaches the critical concentration from below. The results of this scaling analysis suggest the existence of a universal behaviour independent of the sequences and structures of the proteins undergoing phase separation. While we refrain from proposing a theoretical model here, we suggest that any model of protein phase separation should predict the scaling exponents that we reported here from the fitting of experimental measurements of droplet size distributions. Furthermore, based on these observations, we show that it is possible to use the scale invariance to estimate the critical concentration for protein phase separation.

Characterization of Plant based spray dried powders using oil seed proteins and chokeberry extract from wine byproduct

Spray drying is a standard method for preserving bioactive ingredients and enhancing their storage stability. This study aimed to produce entirely plant-based spray-dried powders by using hemp, canola, and flax seed proteins, combined with maltodextrin, as wall material, while chokeberry extract from wine waste served as core material. We conducted a thorough analysis of the oil-seed proteins, examining their nitrogen solubility index, emulsification, and foaming capacities. The encapsulation process was evaluated based on its yield and efficiency. The spray-dried powders were further assessed through colour analysis, particle morphology and size distribution, hygroscopicity, and storage stability measurements. The encapsulation yield with oil-seed proteins ranged from 75.0 ± 6.2 to 78.5 ± 1.3%, and the efficiency from 58.4 ± 0.8 to 77.5 ± 1.9%. These plant-based spray-dried powders exhibited similar colour parameters, morphology, and stability to those of whey protein powders. The study highlights the significant potential of oil-seed proteins in producing plant-based spray-dried powders.

Human milk fat globule size distributions: Comparison between laser diffraction and 3D confocal laser scanning microscopy

Milk fat globules (MFGs) in human milk provide energy to breastfed infants and support infant development. Accurate measurements of MFG size distributions are important to better understand MFG function and origin, as well as the influence of MFG size on milk composition analysis methods. Nevertheless, commonly used laser diffraction systems have never been thoroughly validated for size distribution measurements in human milk. Here, we introduce a new method for determining the size distribution of milk fat globules in human milk, using 3D confocal laser scanning microscopy (CLSM) in combination with fluorescent labeling of MFGs. We validate and compare 3D CLSM to laser diffraction (Mastersizer 2000, Malvern Panalytical), using polystyrene microsphere size standards. Next, we apply both methods to evaluate MFG size distributions in human milk. We show that 3D CLSM can be used to obtain more accurate size distributions between 500 nm and 10 μm compared to laser diffraction. Importantly, MFG size distributions obtained with 3D CLSM contain no secondary population around 1 μm, in contrast to laser diffraction measurements. This suggests that the bimodal MFG distribution obtained by laser diffraction can be an artifact of the built-in fitting algorithm, instead of an actual feature of human milk. This work demonstrates that care should be taken when interpreting size distributions of MFGs measured with laser diffraction and that 3D CLSM is an accurate alternative for measuring size distributions in lactation and dairy research.

Long-range transport of coarse mineral dust: an evaluation of the Met Office Unified Model against aircraft observations

Abstract. Coarse mineral dust particles have been observed much further from the Sahara than expected based on theory. They have impacts different to finer particles on Earth's radiative budget, as well as carbon and hydrological cycles, though they tend to be under-represented in climate models. We use measurements of the full dust size distribution from aircraft campaigns over the Sahara, Canaries, Cabo Verde and Caribbean. We assess the observed and modelled dust size distribution over long-range transport at high vertical resolution using the Met Office Unified Model, which represents dust up to 63.2 µm diameter, greater than most climate models. We show that the model generally replicates the vertical distribution of the total dust mass but transports larger dust particles too low in the atmosphere. Importantly, coarse particles in the model are deposited too quickly, resulting in an underestimation of dust mass that is exacerbated with westwards transport; the 20–63 µm dust mass contribution between 2 and 3.7 km altitude is underestimated by factors of up to 11 in the Sahara, 140 in the Canaries and 240 in Cabo Verde. In the Caribbean, there is negligible modelled contribution of d > 20 µm particles to total mass, compared to 10 % in the observations. This work adds to the growing body of research that demonstrates the need for a process-based evaluation of climate model dust simulations to identify where improvements could be implemented.

On the reliability of image analysis for bubble size distribution measurements in electrolyte solutions in stirred reactors

The translation of chemical processes from laboratory to industrial scale is crucial for the effective and sustainable implementation of new technologies. This transition presents significant challenges, particularly in multiphase systems where variations in physical chemistry can complicate scale-up efforts. A key aspect of this challenge is understanding bubble dynamics in gas-liquid systems, which are pivotal in processes such as hydrogen production and CO2 absorption. Bubble size significantly influences mass transfer rates and process efficiency, necessitating accurate measurement methods. A factorial design approach was employed to assess the sensitivity of results to key parameters. The findings provide quantitative guidelines for optimizing image analysis techniques and improving the accuracy of bubble size measurements in diverse operational conditions. This work advances the understanding of bubble dynamics in gas-liquid systems and offers practical insights for refining measurement techniques, ultimately supporting more effective scale-up of chemical processes.

Dependence of aerosol-borne influenza A virus infectivity on relative humidity and aerosol composition.

We describe a novel biosafety aerosol chamber equipped with state-of-the-art instrumentation for bubble-bursting aerosol generation, size distribution measurement, and condensation-growth collection to minimize sampling artifacts when measuring virus infectivity in aerosol particles. Using this facility, we investigated the effect of relative humidity (RH) in very clean air without trace gases (except ∼400 ppm CO2) on the preservation of influenza A virus (IAV) infectivity in saline aerosol particles. We characterized infectivity in terms of 99%-inactivation time, t 99, a metric we consider most relevant to airborne virus transmission. The viruses remained infectious for a long time, namely t 99 > 5 h, if RH < 30% and the particles effloresced. Under intermediate conditions of humidity (40% < RH < 70%), the loss of infectivity was the most rapid (t 99 ≈ 15-20 min, and up to t 99 ≈ 35 min at 95% RH). This is more than an order of magnitude faster than suggested by many previous studies of aerosol-borne IAV, possibly due to the use of matrices containing organic molecules, such as proteins, with protective effects for the virus. We tested this hypothesis by adding sucrose to our aerosolization medium and, indeed, observed protection of IAV at intermediate RH (55%). Interestingly, the t 99 of our measurements are also systematically lower than those in 1-μL droplet measurements of organic-free saline solutions, which cannot be explained by particle size effects alone.

Preparation of α-zein loaded with baicalincomposites: A study on their in vitro simulated digestive behavior and molecular dynamics simulation

In order to improve the bioavailability of baicalin, this article prepared for α-zein loaded with baicalin composites (α-zein@BA) by pH driven method and they were characterized using scanning electron microscopy, infrared spectroscopy, and measurement of particle size distribution in water solution phase techniques. The digestive behavior and antioxidant activity of composites before and after simulating gastrointestinal fluid in vitro were studied as well. At the same time, molecular dynamics simulation techniques were used to reveal the molecular mechanism behind the formation of the composite between the two. The results indicated that the composites of α-zein@BA were observed to be approximately spherical under a scanning electron microscope, and their particle size was mainly distributed in the range of 94.55-145.10 μm in aqueous solution, whose encapsulation efficiency of baicalin was (86.61 ± 0.71) %. Infrared spectroscopy analysis indicated that α-zein and baicalin mainly formed complexes through hydrogen bonding, electrostatic and hydrophobic interactions. The measurement results of baicalin residue in simulated digestion of gastric and intestinal fluids in vitro are as follows: α-zein@BA > Baicalin, while both significantly increased in the gastric digestion stage (P < 0.05) and significantly decreased in the intestinal digestion stage (P < 0.05). Molecular dynamics simulation studies have shown that baicalin has a promoting effect on protein structural stability, and protein 158SER and GLN196 were mainly formed hydrogen bonds with it, while hydrophobic interactions were mainly manifested between non-polar amino acids such as PHE201 and PRO200. This study indicates that α-zein and baicalin can form stable composites, improving the bioavailability of baicalin.

In situ optical measurement of particles in sediment plumes generated by a pre-prototype polymetallic nodule collector

This study presents in situ, high-resolution optical measurements of particle size distributions (PSD) within sediment plumes generated by a pre-prototype deep seabed nodule collector vehicle operating in the abyssal Pacific Ocean. These measurements were obtained using a cutting-edge instrument, the LISST-RTSSV sensor. The data collected in situ reveal marked differences compared to previously reported laboratory-based, ex situ measurements. The grain size and other key particle shape characteristics are found to be dependent on multiple factors, including the collector vehicle maneuvers, the time elapsed following sediment discharge, and the complex hydrodynamic processes that generate the sediment in suspension. Significantly, the PSD from a highly complex succession of straight-line maneuvers converges to that of the canonical case of a simple straight-line driving maneuver within a timescale of ten minutes. Our results underscore the importance of parameterizing sediment plume transport models based on well-informed, comprehensive PSDs of detrained suspended sediment measured in situ at adequate timescales and in regions no longer strongly influenced by active and complex hydrodynamic processes.

Synthesis of perylene‐PEO hyperdispersants for aqueous graphene dispersion

AbstractGraphene, with excellent thermal conductivity, electrical and corrosion shielding performance has great application potential in the fields of heat dissipation coating, conductive agent and anticorrosion composite coatings. However, due to its large specific surface area, resulting strong aggregation behavior limits its application. Herein, the hyperdispersants with perylene anchoring groups are synthesized through the amidation coupling reaction between diacid anhydride and polyetheramine. The branching degree and length of hydrophilic chains on hyperdispersant are revealed to be the very important factors to affect the dispersion stability of aqueous graphene dispersion. The hyperdispersant with a single hydrophilic chain and the molecular weight 2000 of polyetheramine has the excellent dispersal activity discovered by Rheology, particle size distribution and Raman measurements. The possible mechanism is the strongest anchoring effect of perylene on graphene surface and thus achieving in best effective spatial exclusion stabilization effect of hydrophilic chains.

Soluble mineral flotation paradox: Improved recovery with no sign of collector adsorption on minerals signifies colloidal attraction between bubble-bound collector colloids and mineral particles

Froth flotation uses air bubbles to separate mineral particles based on the difference in mineral surface hydrophobicity. Collectors are needed to selectively hydrophobize the surface of targeted minerals to augment the difference in surface hydrophobicity between wanted minerals and unwanted ones. Here, we showed that this classical (well-established) principle fails to describe the flotation of water-soluble minerals. Our systematic micro-flotation tests using soluble minerals (NaCl and KCl crystals) in brines and three popular collectors (dodecylamine hydrochloride, sodium dodecylsulfate, and sodium laurate) showed a substantial flotation recovery of the salt minerals without detected collector adsorption at the mineral surfaces by X-ray photoelectron spectroscopy (XPS). Complementary particle size distribution measurement indicated the occurrence of sub-micron collector colloids in saturated brines. Moreover, the flotation recovery agreed well with the measured contact angle, suggesting the attraction between bubble-bound collector colloids and salt crystal surfaces. These paradoxical results signify a new principle underlying the flotation of soluble minerals, i.e., the selective colloidal attraction between bubble-bound collector colloids and salt particles enables the flotation separation of soluble minerals.

Measurement report: In situ vertical profiles of below-cloud aerosol over the central Greenland Ice Sheet

Abstract. Surface radiative cooling in polar regions can generate persistent stability in the atmospheric boundary layer. Stable layers below clouds can decouple the cloud layer from the near-surface environment. Under these conditions, surface aerosol measurements are not necessarily representative of the near-cloud or intra-cloud aerosol populations. To better understand the variability in the vertical structure of aerosol properties over the central Greenland Ice Sheet, in situ measurements of aerosol particle size distributions up to cloud base were made at Summit Station in July and August 2023. These measurements identified distinct vertical aerosol layers between the surface- and cloud-base-associated thermodynamic decoupling layers. Such decoupling layers occur 49 % of the time during the summer in central Greenland, suggesting that surface aerosol measurements are insufficient for describing the cloud-relevant aerosol population half of the time. Experience during this first measurement season demonstrated the ability of a tethered-balloon platform to operate effectively under icing conditions and at low surface pressure (&lt; 680 hPa). The results presented here illustrate the value of vertically resolved in situ measurements of aerosol properties in developing a nuanced understanding of the aerosol effects on cloud properties in polar regions.

Isolation and Characterization of Cellulose Nanofibrils (CNF) from Dates by-Product via Citric Acid Hydrolysis

Industrial residues that are not optimally utilized are removed by burning, landfilling, or dumping, which can threaten the environment and health. In fact, part of this agro-industrial waste still has content that has the potential to become raw material for value-added other industries. Dates by-product as residue of the fiber-rich fruit industry have the potential to be a source of nanocellulose. This study aims to obtain nanofibril cellulose (CNF) isolates from dates by-product via citric acid hydrolysis, and investigate the effect of acid concentration on the unknown dates by-product CNF isolate characteristics. Pretreatment such as delignification and bleaching is needed to obtain cellulose isolate with high purity. Furthermore, acid hydrolysis, centrifugation, and sonication are performed to obtain CNF. CNF isolates are characterized by the analysis of particle size distribution, morphology, and crystallinity. Analysis of functional groups and lignocellulose content test confirm that lignin and hemicellulose are degraded during isolation. The particle size distribution measurement shows that the greater the acid concentration, the smaller the CNF size and the better the size uniformity. The morphology of the CNF obtained is net-like fibers. The degree of crystallinity shown decreases with increasing acid concentration. This study revealed that different citric acid concentrations can result in different characteristics of CNF isolates.

Novel CD44-Targeted Albumin Nanoparticles: An Innovative Approach to Improve Breast Cancer Treatment.

This study introduces novel CD44-targeted and redox-responsive nanoparticles (FNPs), proposed as doxorubicin (DOX) delivery devices for breast cancer. A cationized and redox-responsive Human Serum Albumin derivative was synthesized by conjugating Human Serum Albumin with cystamine moieties and then ionically complexing it with HA. The suitability of FNPs for cancer therapy was assessed through physicochemical measurements of size distribution (mean diameter of 240 nm), shape, and zeta potential (15.4 mV). Nanoparticles possessed high DOX loading efficiency (90%) and were able to trigger the drug release under redox conditions of the tumor environment (55% release after 2 h incubation). The use of the carrier increased the cytotoxic effect of DOX by targeting the CD44 protein. It was shown that, upon loading, the cytotoxic effect of DOX was enhanced in relation to CD44 protein expression in both 2D and 3D models. DOX@FNPs significantly decrease cellular metabolism by reducing both oxygen consumption and extracellular acidification rates. Moreover, they decrease the expression of proteins involved in the oxidative phosphorylation pathway, consequently reducing cellular viability and motility, as well as breast cancer stem cells and spheroid formation, compared to free DOX. This new formulation could become pioneering in reducing chemoresistance phenomena and increasing the specificity of DOX in breast cancer patients.

Nanodosimetric investigation of the track structure of therapeutic carbon ion radiation part 1: measurement of ionization cluster size distributions

At the Heidelberg Ion-Beam Therapy Center, the track structure of carbon ions of therapeutic energy after penetrating layers of simulated tissue was investigated for the first time. Measurements were conducted with carbon ion beams of different energies and polymethyl methacrylate (PMMA) absorbers of different thicknesses to realize different depths in the phantom along the pristine Bragg peak. Ionization cluster size (ICS) distributions resulting from the mixed radiation field behind the PMMA absorbers were measured using an ion-counting nanodosimeter. Two different measurements were carried out: (i) variation of the PMMA absorber thickness with constant carbon ion beam energy and (ii) combined variation of PMMA absorber thickness and carbon ion beam energy such that the kinetic energy of the carbon ions in the target volume is constant. The data analysis revealed unexpectedly high mean ICS values compared to stopping power calculations and the data measured at lower energies in earlier work. This suggests that in the measurements the carbon ion kinetic energies behind the PMMA absorber may have deviated considerably from the expected values obtained by the calculations. In addition, the results indicate the presence of a marked contribution of nuclear fragments to the measured ICS distributions, especially if the carbon ion does not cross the target volume.

The change rule of lipid oxidation and hydrolysis driven via water in Antarctic krill oil: Based on association colloid formation

The residual water and amphiphilic compounds such as phospholipids in bulk oil can form reverse micelles, which affect oxidative stability. In this study, the Antarctic krill oil (AKO) samples with different water contents were subjected to accelerated storage. During storage, AKO exhibited oxidative changes, manifested as increased POV, TBARS values, and volatile compound levels but decreased PUFA percentages. Meanwhile, AKO underwent hydrolysis, evidenced by decreased PC, PE, and TG contents but increased FFA contents. Moreover, the degree of lipid oxidation and hydrolysis is dose-dependent with water added. Cryogenic scanning electron microscopy imaging and micelle size distribution measurement proved the presence of reverse micelle, and their size and interfacial area improved with increased water contents. Correlation analysis suggested that lipid oxidation and hydrolysis positively correlated with the size and interfacial area of reverse micelle. Therefore, it is speculated that the oil-water interface may be the site of lipid oxidation and hydrolysis.

Enhancing emulsion stability and adsorption of Pickering emulsions using alkylated cellulose nanofibers

Cellulose nanofibers (CNFs) extracted from plant cell walls form a three-dimensional network in water and stabilize the dispersion of droplets, which are used as emulsion stabilizers. In this study, four types of alkyl-grafted CNFs (ACNFs) with different lengths of dialkyl chains (diC4, diC6, diC8, and diC10) were synthesized by the surface modification of 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO)-oxidized CNF (TOCNF) to improve the stability of oil-in-water Pickering emulsions (PEs). The ACNF-stabilized emulsions with a 20/80 ratio of oil/water were prepared using two different oils (olive oil and eucalyptus oil) and the ACNF 1.0 % dispersion, and the changes over time were investigated at approximately 25 °C. Compared to TOCNF, the ACNFs provided more stable olive oil-PE (o-PE) and eucalyptus oil-PE (e-PE) although the stabilization behaviors of o-PE and e-PE differed. Olive oil, which contained rich long-chain fatty acids, was more likely to interact with the ACNFs, thereby promoting the interfacial adsorption of oil droplets. On the other hand, eucalyptus oil is mainly composed of 1,8-cineole and does not have alkyl chains, so the interaction with the ACNFs was weak and therefore, sufficient interfacial adsorption could not be obtained. The results of the particle size distribution and viscosity measurements also showed that the ACNFs contributed significantly to the stabilization of o-PE. Based on the overall experimental results, it was determined that the diC6-ACNF gave the most significant stability improvement. Therefore, we designed an alkylated CNF that mimics diC6-ACNF for MD simulations. MD simulations showed that hydrophobic modification created a hydrophobic interaction between the alkyl chain and dodecane molecules as the oil, leading to the enhancing adsorption of ACNF at the oil droplet interfaces.