Search Results (14)

Unlike medicinal products (MPs), dietary supplements (DSs), foods for special medical purposes (FSMPs) and fortified foods (FFs) available on the Polish market are not required to meet pharmacopoeial quality standards. Dose uniformity testing, a pharmacopoeial requirement for MPs, confirms both the accuracy of the declared dose and consistency between individual doses. As consumption of DSs, FSMPs, and FFs continues to increase, particularly among vulnerable populations, ensuring consistent intake of essential nutrients becomes increasingly important. Therefore, adapting pharmacopoeial dose uniformity criteria to elemental analysis may provide an additional quality assessment tool beyond the percentage of the label claim. Accordingly, this study aimed to (1) validate a multi-element High-Resolution Inductively Coupled Plasma Optical Emission Spectrometry (HR-ICP-OES) method for assessing dose uniformity and (2) evaluate the uniformity of elemental doses in one DS and four FSMPs according to pharmacopoeial guidelines, with MPs included as reference materials. To achieve this, the key parameters of the HR-ICP-OES measurement methodology were defined to ensure reliable results, and the uniformity of the doses of the seven preparations was determined by establishing a pharmacopoeial acceptance value. Although HR-ICP-OES is useful for multi-element analysis of products, limitations have been identified relating to chemical and spectral interference, and to the analysis of selenium at low levels. Of the DSs and FSMPs analysed, none complied with the pharmacopoeial requirements for uniformity. Full article

Molting is an important biological and physiological stage in penguins, influenced by environmental and nutritional factors. Feather composition analysis before and after molting can consequently place boundaries on element bioaccumulation and excretion. We quantified and compared elemental concentrations in African penguin (Spheniscus demersus) feathers collected pre- and post-molt across three zoos to evaluate how molt stage and zoo-specific conditions influence feather elemental composition. Feathers were retrieved from individual penguins at Zoom Torino (Italy), Overloon ZooParc (Netherlands), and Zoo Magdeburg (Germany). Quantification of elemental concentrations were performed by analytical methods, with both ICP-OES and HR-ICP-MS techniques. A statistical approach involving MANOVA and factorial analysis helped identify important trends. Pre-molt features had more variability than post-molt, with both showing significant differences in elemental concentrations. Factorial analysis showed geogenic trends in Mg, Sr, and Ni trends as well as anthropogenic trends in Pb. While Na and K differed among all treatment groups, this likely points to physiological adaptations in response to increased demand during feather regrowth. Additionally, inter-zoo comparisons highlighted distinct elemental profiles linked to local environmental and dietary conditions, particularly in Zoo Magdeburg, where Na levels were markedly elevated. This study highlights the influence of environmental and dietary conditions on feather composition during molt, offering insights for improving captive penguin welfare and broader ecological implications related to climate change and pollution. Full article

This article presents the results of an analysis of ceramics from archeological sites. The main goal of the study was to determine the elemental composition of ceramics using XRF. This study was conducted in two stages. The first stage involved the analysis of complete vessels from the museum exhibition. The second involved the interpretation of the results obtained from the first stage. In the second stage, 30 samples obtained by dividing a single fragment of a ceramic vessel were analyzed. The results (results scattered due to material heterogeneity) were compared with the results of analyses of a large group of ceramic samples from a similar period. To supplement the information about the ceramic material studied, destructive analyses were also performed (after grinding the aforementioned 30 samples), namely mineral composition using FTIR (to determine the raw materials) and iron speciation using UV-Vis and HPLC-ICP hrOES (to determine the firing method). The results obtained indicated that limiting the research to the most-used non-destructive procedures in archaeometry can lead to misinterpretation. Although the presented study concerned archaeological objects, it can be considered in the context of research on other materials. Full article

Fundamental research, exploration, extraction, and metallurgical studies of rare earth elements (REEs) require the use of analytical techniques. Recently, emerging developments of analytical instrumentation for REEs have taken place, with some of them having shrunk in size, becoming handheld devices. The Flame and Graphite Furnace AAS, ICP-OES, and MP-AES are standard laboratory techniques used for the analysis of REEs. ICP-MS, ICP-MS/MS, ICP-TOF-MS, HR-ICP-MS, MH-ICP-MS, and MC-ICP-MS are popular techniques for REE analysis thanks to their ultrahigh sensitivity, minimal interference effects, and broad applicability. The INAA, XRF, LIBS, and LA-based ICP-MS techniques are widely employed for the direct analysis of solid samples. The TIMS, SIMS, and SHRIMP are common techniques used for dating isotopic REE deposits. The portable XRF, LIBS, and Raman spectrometer devices can perform on-the-spot in situ analysis, which may help make speedy decisions in the exploration study of REEs. Currently, hyperspectral remote sensing platforms, such as handheld, drone, and satellite-based devices, are preferred for the exploration of REEs due to their cost-effectiveness, which enables the coverage of large areas in a limited amount of time. The use of microanalytical sensors installed on remotely operated vehicles has been successfully applied in analyzing rich REE-bearing deposits in the deep sea. In general, this review provides in-depth information on all essential aspects, from analytical instruments to cutting-edge developments in the analysis of REE-bearing resources. Full article

Kutno is a picturesque city in central Poland, known for extensive rose breeding worldwide. Soil samples and rose petals were collected from 13 locations in the city and characterized by diverse environments. This allowed determining the response of plants to changing cultivation conditions. Rose petals have found a wide range of applications. They are used in the food, pharmaceutical and cosmetic industries. The aim of the research was to assess the contents of Cu, Zn, Cd, Ni, Pb and Cr in soils and their accumulation in rose petals. Samples were subjected to the microwave mineralization process using a mixture of concentrated HCl and HNO₃. The metal contents in the soil and roses were determined by HR-CS-AAS and ICP-OES, respectively. Roses are usually cultivated in soils with a limited mobile fraction of heavy metals. In these unfavorable conditions, flower petals can absorb heavy metals substantially. Petals of roses cultivated for cosmetic, pharmaceutical or food purposes should be tested for heavy metal content. This study indicates that toxic metals are blocked at the root zone, and their transport to the above-ground parts is severely hampered. Nevertheless, metals related to the photo-synthesis process (Zn, Cu) are more intensively taken up by roses, while the uptake of toxic metals is partially inhibited. Full article

Phosphorylated cellulose can be an intrinsic flame retardant and a promising alternative for halogenated fire inhibitors. In this study, the mixture of di-ammonium hydrogen phosphate (DAP) and urea (U), containing phosphate and nitrogen groups, was applied to attain fire inhibitor properties. Functional groups of cellulose were grafted with phosphorous by keeping the constant molar ratio of 1/1.2/4.9 between anhydroglucose units of cellulose/DAP/U in different concentrations of bleached kraft pulp. Phosphorus concentrations were determined using the ICP hrOES method, and paper sheets were made using the Rapid Köthen apparatus. The tensile strength of phosphorylated cellulose increased twice compared with unmodified cellulose when the phosphorous concentration increased to 10,000 g/kg. An increase in the tensile index comes from the higher freeness of pulp and cross-linking of the phosphorous group between cellulose fibers. Remarkable fire retardancy effects were achieved in cellulose concentrations above 5 wt%. The raised phosphorous concentration above 10,000 g/kg due to the phosphorylation process caused the formation of a char layer on a cellulose surface and the nonflammable gas emission. That effect was indirectly confirmed by reducing the combustion temperature and HRR by 50 and 45%, respectively. Due to increasing phosphorus concentration in cellulose sheets, cellulose’s fire and strength properties increased significantly. Full article

The use of analytical techniques is important and critical in all areas related to REE, such as basic fundamental research, exploration, mining, extraction, and metallurgical activities at different stages by different industries. At every stage of these activities, rock, ore, minerals, and other related materials have to be analyzed for their REE contents in terms of elemental, isotopic, and mineralogical concentrations using different analytical techniques. Spectacular developments have taken place in the area of analytical instrumentation during the last four decades, with some of them having shrunk in size and become handheld. Among laboratory-based techniques, F-AAS, GF-AAS, ICP-OES, and MP-AES have become very popular. Because of high sensitivity, fewer interference effects, and ease of use, ICP-MS techniques, such as quadrupole ICP-MS, ICP-MS/MS, ICP-TOF-MS, MH-ICP-MS, HR-ICP-MS, and MC-ICP-MS, with both solution nebulization as well as direct solid analysis using laser ablation sample introduction methods, have become more popular for REE analysis. For direct analysis of solids, INAA, XRF, and LIBS techniques, as well as LA-based ICP-MS techniques, are being extensively utilized. The LIBS technique in particular requires little to no sample preparation. TIMS, SIMS, and SHRIMP techniques are being used for isotopic as well as dating REE depots. Portable analytical techniques, such as pXRF, pLIBS, and Raman spectrometers are able to perform in situ analysis even in the field, helping to make fast decisions during exploration studies. At present, hyperspectral remote sensing techniques including handheld, drone, and satellite-based techniques have become very popular in REE exploration studies because of their ability to cover larger areas in a limited time and, thus, became very cost-effective. Deployment of microanalytical devices/sensors mounted in remotely operated vehicles (ROV) is being successfully utilized in detecting REE-rich deposits in the deep oceans. Providing updated in-depth information on all these important aspects with suitable examples, especially from the point of view of REE research studies is the focal point of this review article. Full article

The optimization and application of a new hyphenated procedure for iron ionic speciation, i.e., high performance liquid chromatography (HPLC) with short cation–exchange column (50 mm × 4 mm) coupled to high resolution inductively coupled plasma optical emission spectrometry (ICP hrOES), is presented in this paper. Fe(III) and Fe(II) species were separated on the column with the mobile phase containing pyridine–2,6–dicarboxylic acid (PDCA). The total time of the analysis was approx. 5 min, with a significantly low eluent flow rate (0.5 mL min⁻¹) compared to the literature. Additionally, a long cation-exchange column (250 mm × 4.0 mm) was used as reference. Depending on the total iron content in the sample, two plasma views were chosen, e.g., an attenuated axial (<2 g kg⁻¹) and an attenuated radial. The standard addition method was performed for the method’s accuracy studies, and the applicability was presented on three types of samples: sediments, soils, and archaeological pottery. This study introduces a fast, efficient, and green method for leachable iron speciation in both geological and pottery samples. Full article

Cerium oxide nanoparticles (CeO₂ NPs) and zinc oxide nanoparticles (ZnO NPs) are emerging pollutants that are likely to occur in the contemporary environment. So far, their combined effects on terrestrial plants have not been thoroughly investigated. Obviously, this subject is a challenge for modern ecotoxicology. In this study, Pisum sativum L. plants were exposed to either CeO₂ NPs or ZnO NPs alone, or mixtures of these nano-oxides (at two concentrations: 100 and 200 mg/L). The plants were cultivated in hydroponic system for twelve days. The combined effect of NPs was proved by 1D ANOVA augmented by Tukey’s post hoc test at p = 0.95. It affected all major plant growth and photosynthesis parameters. Additionally, HR-CS AAS and ICP-OES were used to determine concentrations of Cu, Mn, Fe, Mg, Ca, K, Zn, and Ce in roots and shoots. Treatment of the pea plants with the NPs, either alone or in combination affected the homeostasis of these metals in the plants. CeO₂ NPs stimulated the photosynthesis rate, while ZnO NPs prompted stomatal and biochemical limitations. In the mixed ZnO and CeO₂ treatments, the latter effects were decreased by CeO₂ NPs. These results indicate that free radicals scavenging properties of CeO₂ NPs mitigate the toxicity symptoms induced in the plants by ZnO NPs. Full article

This study aimed at investigating both the surface and bulk modifications occurring on fibrous erionite during leaching in a mimicked Gamble’s solution (MGS) at pH of 4.5 and T = 37 °C, up to one month of incubation. Samples were characterized by a multi-analytical approach: field-emission scanning electron microscopy (FE-SEM) was employed to investigate the morphological changes of both pristine and reacted fibres, inductively coupled plasma optical emission spectrometry (ICP-OES) was used to measure the concentration of the released cations; X-ray photoelectron spectroscopy (XPS) was exploited for highlighting possible modifications of surface chemistry; X-ray powder diffraction (XRPD) and high-resolution transmission electron microscopy (HR-TEM) were applied aiming to get information on the structural state of the fibres following the incubation. ICP results integrated with those obtained by both bulk- and surface-chemical characterization highlighted that erionite binds Na especially in the first 24 h of sample incubation in the MGS, following ion exchange with the extra framework cations, in particular Ca. Moreover, our new results show that the Na binding process caused structural modifications with the migration of Na toward the Ca2 site and redistribution of the cations within the erionite cage. TEM investigation pointed out that the interaction between erionite and MGS results in the formation of a new surface amorphous layer with an irregular lobate pattern on an earlier surface weathered layer. However, the silicate framework is not weakened by incubation in the MGS at acidic pH. In addition, on the basis of the Si release normalized to the mineral surface area, fibrous erionite resulted significantly more biodurable than amphibole asbestos. Notably, considering the primary role played by biodurability in inducing pathogenicity, this result certainly supports in vivo observations showing that erionite is much more tumorigenic than asbestos. Moreover, the ions released by erionite when immersed in MGS may trigger biological effects, such as those on lipid packing and membrane permeability. On this basis, we expect a regulatory definition that would provide protection from this carcinogenic fibre. Full article

The aim of the study was to establish the influence of a co-precipitation agent (i.e., NaOH–immediate precipitation; hexamethylenetetramine/urea–gradual precipitation and growth of nanostructures) on the properties and catalytic activity of as-synthesized Au-CeO₂ nanocomposites. All catalysts were fully characterized with the use of XRD, nitrogen physisorption, ICP-OES, SEM, HR-TEM, UV-vis, XPS, and tested in low-temperature oxidation of benzyl alcohol as a model oxidation reaction. The results obtained in this study indicated that the type of co-precipitation agent has a significant impact on the growth of gold species. Immediate co-precipitation of Au-CeO₂ nanostructures with the use of NaOH allowed obtainment of considerably smaller and more homogeneous in size gold nanoparticles than those formed by gradual co-precipitation and growth of Au-CeO₂ nanostructures in the presence of hexamethylenetetramine or urea. In the catalytic tests, it was established that the key factor promoting high activity in low-temperature oxidation of benzyl alcohol was size of gold nanoparticles. The highest conversion of the alcohol was observed for the catalyst containing the smallest Au particle size (i.e., Au-CeO₂ nanocomposite prepared with the use of NaOH as a co-precipitation agent). Full article

Dimethyl disulfide (DMDS, CH₃SSCH₃) is an odorous and harmful air pollutant (volatile organic compound (VOC)) causing nuisance in urban areas. The abatement of DMDS emissions from industrial sources can be realized through catalytic oxidation. However, the development of active and selective catalysts having good resistance toward sulfur poisoning is required. This paper describes an investigation related to improving the performance of Pt and Cu catalysts through the addition of Au to monometallic “parent” catalysts via surface redox reactions. The catalysts were characterized using ICP-OES, N₂ physisorption, XRD, XPS, HR-TEM, H₂-TPR, NH₃-TPD, CO₂-TPD, and temperature-programmed ¹⁸O₂ isotopic exchange. The performance of the catalysts was evaluated in DMDS total oxidation. In addition, the stability of a Pt–Au/Ce–Al catalyst was investigated through 40 h time onstream. Cu–Au catalysts were observed to be more active than corresponding Pt–Au catalysts based on DMDS light-off experiments. However, the reaction led to a higher amount of oxygen-containing byproduct formation, and thus the Pt–Au catalysts were more selective. H₂-TPR showed that the higher redox capacity of the Cu-containing catalysts may have been the reason for better DMDS conversion and lower selectivity. The lower amount of reactive oxygen on the surface of Pt-containing catalysts was beneficial for total oxidation. The improved selectivity of ceria-containing catalysts after the Au addition may have resulted from the lowered amount of reactive oxygen as well. The Au addition improved the activity of Al₂O₃-supported Cu and Pt. The Au addition also had a positive effect on SO₂ production in a higher temperature region. A stability test of 40 h showed that the Pt–Au/Ce–Al catalyst, while otherwise promising, was not stable enough, and further development is still needed. Full article

Mono- and bimetallic systems of Ag, Fe, and Ag–Fe exchanged in sodium mordenite zeolite were studied in the reaction of NO reduction. The transition metal cations Ag and Fe were introduced by ion exchange method both at room temperature and 60 °C; modifying the order of component deposition in bimetallic systems. These materials were characterized by Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES), ultraviolet-visible spectroscopy (UV-Vis), X-Ray photoelectron Spectroscopy (XPS) and High-resolution transmission electron microscopy (HR-TEM). The XPS and UV–Vis spectra of bimetallic samples revealed that under certain preparation conditions Ag⁺ is reduced with the participation of the Fe²⁺/Fe³⁺ ions transition and is present in the form of a Ag reduced state in different proportions of Ag_m clusters and Ag⁰ NPs, influenced by the cation deposition order. The catalytic results in the NO reduction reaction using C₃H₆/CO under an oxidizing atmosphere show also that the order of exchange of Ag and Fe cations in mordenite has a strong effect on catalytic active sites for the reduction of NO. Full article

In this work we report the effects of support structural properties and its modification with some metal oxides modifiers on the catalytic behavior of Au catalysts in the total CO oxidation at 20 °C. Au catalysts were supported on mesoporous silica materials (MSM) having different structural properties: Channel-like (SBA-15), cage-like (SBA-16), hexagonal (HMS), and disordered (DMS-1) structures. The effect of the modifier was evaluated by comparison of the catalytic response of the SBA-15-based catalysts modified with MgO, Fe₂O₃, TiO₂, and CeO₂. The chemical, structural, and electronic properties of the catalysts were investigated by a variety of techniques (metal content analysis by ICP-OES, N₂ physisorption, XRD, UV-vis DRS, DRIFTS of adsorbed CO and OH regions, oxygen storage capacity (OSC), HR-TEM, and XPS). The activity of calcined catalysts in the CO oxidation reaction were evaluated at steady state conditions, at 20 °C, atmospheric pressure, and when using, as feed, a 1%CO/1%O₂/98% gas mixture. The work clearly demonstrated that all Au catalysts supported on the mesoporous silicas modified with metal oxides were more active than the Au/SBA-15 and Au/MgO reference ones. The support structural properties and type of dopant were important factors influencing on the catalyst behavior. Concerning the support textural properties, it was found that the HMS substrate with the wormhole-structure offers better porosity and specific surface area than their silica counterparts having channel-like (SBA-15), cage-like (SBA-16), and disordered (DMS-1) mesoporous structures. Concerning the effect of modifier, the best catalytic response was achieved with the catalysts modified with MgO. After activation by calcination at 200 °C for 4 h, the Au/MgO/HMS catalyst exhibited the best catalytic performance, which was ascribed to the combined effects of the best structural properties, a large support oxygen storage capacity and homogeneous distribution of gold particles on the support (external and inner). Implications of the type of active sites (Au¹⁺ or Au⁰), support structural properties and role of modifier on the catalytic activity are discussed. Full article