Inductively Coupled Plasma Mass Spectrometry Analysis Research Articles

Removal of Cadmium from Public Smoking area Soil using indoor Plants and Electrical Grounding

Objectives : In this study, the absorption of heavy metals in the soil from smoking areas using indoor plants and electrical grounding was investigated to increase the utility of indoor plants for soil decontamination.Methods : Soil from plant pots in a smoking area was collected for the experimental plant pot preparations. Some of the prepared pots were connected to electrical ground via an electrode. Kidney beans (<i>Phaseolus vulgaris</i>) were seeded, and their growth were observed. After 30 days of the cultivation, TOC (Total Organic Carbon), and metagenomics profiles in the soil was analyzed. To estimate the behavior of the heavy metals in soil and plants, Cadmium concentrations in the samples were analyzed using ICP-MS (Inductively Coupled Plasma-Mass Spectrometry).Results and Discussion : The connection of the electrical ground to the plant pot induced the rapid growth of plant (48.2 ± 2.3% increase in stem growth), compare to the plant in the pot without the electrical ground. TOC analysis showed that the soil from the grounded pots showed the highest value, compared to the control soil (3.08 ± 1.22%), and the soil from the pot without ground connection (2.3 ± 0.1%). The ICP-MS analysis indicated that the plant body in the grounded pot had the highest cadmium concentration at 0.33 ± 0.018 μg/kg. Using the metagenomic analysis, biomineralization related bacterial species (<i>Nocardioides</i> sp., <i>Streptomyces</i> sp., <i>Sphingomonas</i> sp. etc.) were identified from the grounded soil sample. These results suggested that the indoor plant cultivation with the electrical ground connection as an electrical fertilizer enhances the cadmium absorption by plant, exudate secretion from the plant root, and bacterial flora change in the rhizosphere.Conclusion Cadmium in the soil from the smoking area was absorbed by indoor plant with the electrical ground. Therefore, the application of the electrical ground connection (earth) to the electrically insulated outdoor plant pots might enhance the plant growth rate and physiological activity. This application could be a novel soil decontamination method using plants.

Multivariate Statistical Analysis for the Classification of Sausages Based on Physicochemical Attributes, Using Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS).

Sausage is a convenient food that is widely consumed in the world and in Vietnam. Due to the rapid development of this product, the authenticity of many famous brands has faded by the rise of adulteration. Therefore, in this study, principal component analysis (PCA) was combined with chemical analysis to identify 6 sausage brands. Sausage samples were dried and then ground to a fine powder for both instrumental analyses of attenuated total reflectance-Fourier transform infrared (ATR-FTIR) and inductively coupled plasma-mass spectrometry (ICP-MS). Dried measurements of ATR-FTIR was performed directly on the ZnSe crystal, while elemental data were obtained through microwave digestion before the ICP-MS analysis. Principal component analysis (PCA) within the framework software of XLSTAT and STATISTICA 12 was performed on the spectroscopy and elemental dataset of sausage samples. PCA visualized the distinction of 6 sausage brands on both datasets of ATR-FTIR and ICP-MS. The classification on the spectroscopy profile showed that although more than 90% variation of the dataset was explained on the first two PCs, the difference between several brands was not detected as the distribution of data overlapped with one another. The PCA observation of the elemental composition on PC1 and PC3 has separated the sausage brands into 6 distinctive groups. Besides, several key elements contributed to the brands' identification have been detected, and the most distinctive elements are Na, K, Ca, and Ba. PCA visualization showed the feasibility of the classification of sausage samples from different brands when combined with the results of FT-IR and ICP-MS methods. The experiment was able to differentiate the sausages from the 5 brands using multivariate statistics.

Tetrafluoroboric Acid Digestion for Accurate Determination of Rare Earth Elements in Coal and Fly Ash by ICP-MS Analysis

Coal and coal-related fly ash often contain rare earth elements (REEs) that have the potential to be utilized as valuable mineral resources. Accurately determining the REE content in coal and fly ash is crucial for resource evaluation. The conventional approach involves using hydrofluoric acid (HF) to dissolve silicates and release REEs, which, however, prolongs the digestion process due to the additional step of complexing fluoride ions (F−) with boric acid (H3BO3). Determining the correct amount of H3BO3 for neutralization can be challenging, and in some instances, the binding of fluoride ions with certain lanthanides (Lns) hampers the accurate determination of all 14 naturally occurring rare earth elements in a single digestion batch by inductively coupled plasma mass spectrometry (ICP-MS). In this study, we present an alternative method that achieves the accurate determination of all 14 naturally occurring REEs using tetrafluoroboric acid (HBF4) followed by ICP-MS analysis. This approach eliminates the need for an F− complexing step. We tested this method on certified REE reference materials, including NIST 1632e (coal) and NIST 1633c (fly ash), as well as the REE geological reference material USGS AGV-1 (andesite). Our results demonstrated excellent recovery rates (relative standard deviation, RSD < ±10%), with a correlation coefficient (r2) exceeding 0.99. Using this method, we investigated the concentrations of all 14 REEs in coal and fly ash samples collected from various locations in the southwestern USA. This improved digestion technique streamlines the analysis process and enhances the accuracy of REE determination, facilitating a more comprehensive evaluation of REE-rich coal and fly ash deposits for resource exploration.

Assessment on the Toxic Effects of Chemically Synthesized SPIONs against Model Organisms

The remarkable physicochemical properties of nanomaterials have attracted researchers due to the numerous applications in the field of chemistry, biology, and physics. Despite the various applications, superparamagnetic iron oxide nanoparticles (SPIONs) are harmful to living organisms and to the environment as they are released without any safety testing. In this study, SPIONs were synthesized and further characterized. The aim of the study was to examine the toxicity of synthesized SPIONs against animal models: Zebrafish—Danio rerio, Earthworm—Eudrilus eugeniae, and Drosophila—Drosophila melanogaster through histology using Hematoxylin–Eosin and Prussian Blue staining. The accumulation of SPIONs was further quantified by using Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Through histology images, it was observed that the SPIONs had caused damages and a lower concentration of 0.001–0.002 μg/ml of metal accumulation was detected in the ICP-MS analysis.

Cellular uptake and biotransformation of arsenate by freshwater phytoplankton under salinity gradient revealed by single-cell ICP-MS and CT-HG-AAS

Environmental context Freshwater phytoplankton are involved in the biogeochemical cycling of arsenic within aquatic ecosystems via uptake processes. Rather than determining the mean arsenic content in a population of freshwater phytoplankton, we investigate the heterogeneity of arsenic uptake by single-cell ICP-MS. Our data show that arsenic distribution within a cell population may be highly heterogeneous, measured at the femtogram per cell level, and are affected by species and salinity. Rationale An advanced technique has been developed for analysing intracellular elements at the single-cell level using single-cell inductively coupled plasma mass spectrometry (SC-ICP-MS). Compared with conventional inductively coupled plasma mass spectrometry (ICP-MS) analysis, SC-ICP-MS provides uptake data with greater biological relevance. In this study, the use of SC-ICP-MS enabled the quantification of metal concentrations on an individual cell basis down to the femtogram (fg) per cell level. Methodology Three freshwater phytoplankton cells, namely Staurastrum paradoxum (S. paradoxum), Pediastrum duplex (P. duplex) and Scenedesmus acutus (S. acutus), were incubated in 0.1 µmol L−1 arsenate (AsV) solution for 14 days at varying salinity. Cold trap hydride generator atomic absorption spectrometry (CT-HG-AAS) was used to investigate the biotransformation of arsenate under varying salinity conditions. Results The results reveal that cellular arsenic levels decreased as salinity increased in P. duplex and S. paradoxum but increased in S. acutus. The SC-ICP-MS data, which show uptake of AsV by freshwater phytoplankton, were in good agreement with those produced using ICP-MS analysis. Various arsenic management strategies were seen in the phytoplankton species: P. duplex converted it to methylated forms; S. acutus produced organoarsenicals; and S. paradoxum reduced arsenate (AsV) to arsenite (AsIII) and excreted it. Our study also showed changes in the physiological status of phytoplankton following salt stress and arsenic exposure. Discussion Our results confirm the efficacy of SC-ICP-MS in precisely determining arsenic distribution at the single-cell level and reveal differences in intraspecies mechanisms for arsenic cycling in freshwater ecosystems.

Age dating of liquid 90Sr–90Y sources

In the context of age dating of 90Sr, the selective adsorption of zirconium ions from the mixture with strontium and yttrium by adsorbents based on TiO2 with a chemically modified surface was investigated. The general features of the separation process of strontium, yttrium, and zirconium in batch conditions were determined. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) was used to analyze the initial and residual concentrations of the studied cations. Separation of 90Zr and 90Sr from a liquid source containing 90Sr–90Y using adsorbents based on TiO2 was performed for the first time. The ratio of 90Zr/90Sr was measured, and the age of liquid 90Sr–90Y sources was determined. In addition, we studied the age dating of 90Sr–90Y sources using a combination of liquid-scintillation counting of 90Sr and ICP-MS measurement. The results of both methods – the method of age-dating with the chemical separation of isotopes and the combination of LSC and ICP-MS analysis – agree very well and thus serve for cross-validation. Moreover, the combination of the two methods increases the confidence in the age-dating results of 90Sr–90Y sources.

Mineralogy and elemental geochemistry of pyrite coal-balls, Datong Coalfield, Shanxi Province, China: Implications for differentiation mechanism

The pyrite coal-balls found in No.9 coal of Taiyuan Formation in Dongzhouyao Mine of Datong Coalfield were selected to investigate its mineralogy and elemental geochemistry using optical microscope observation, scanning electron microscopy combined with an energy-dispersive X-ray spectrometer (SEM-EDX), inductively coupled plasma mass spectrometry analysis (ICP-MS), laser ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS), and electron probe micro-analysis (EPMA). Due to the high content of pyrite, the major-element oxides in the coal-ball samples were mainly Fe2O3, with an average of 62.68 %. LA-ICP-MS results showed that coal-balls were enriched in Tl (CC = 32.79), Pb (CC = 9.22), and Mo (CC = 2.07), while the coals in the same layer were enriched in Ga (CC = 5.31), Tl (CC = 3.66), and Li (CC = 2.27). Affinities to S or Fe and the variation of elemental concentration in the environment during the formation of coal-balls were the primary factor of the elemental differentiation between coals and coal-balls, as well as within coal-balls. The coal-balls formed in four stages in a marine-continental transition environment, with Fe from terrestrial sources and S from marine phases, and its physical origin is basically consistent with that of some Carboniferous-Permian coals in the Datong Coalfield. According to the formation sequence and geochemical characteristics, four periods of pyrite coal-balls evolution have been proposed.

Application of MARS-5 and UltraWAVE microwave systems to the digestion of silicate rocks followed by ICP-MS analysis

Two microwave systems MARS-5 and UltraWAVE are compared in the efficiency with regard to the digestion of silicate rocks with subsequent determination of 32 elements (Sc, V, Cr, Co, Ni, Cu, Zn, Rb, Sr, Y, Nb, Ta, Cs, Ba, 14 REE, Hf, Ta, Th, U) by inductively coupled plasma mass spectrometry (ICP-MS). The development of digestion methods and validation of the obtained results has been carried out using international reference materials — basalts BHVO-2 and BCR-2, serpentinite UB-N and peridotite JP-1. Microwave digestion included a two-stage treatment of samples with a mixture of concentrated acids HF, HNO3, HCl in MARS-5 (T = 190°C, P = 20 bar) and UltraWAVE (T = 240°C, P = 80 bar) with distillation of excess fluorides in the form of SiF4 between microwave digestion stages. The determination of concentrations in the obtained solutions was carried out on a high-resolution mass spectrometer ELEMENT in low and medium resolution according to external calibration with the internal standard (In), taking into account the acid composition of the analyzed solutions. The detection limits of the analytes after acid digestion in MARS-5 and UltraWAVE are comparable and provide the determination of all specified elements, except for Ta in JP-1. The use of the developed sample preparation procedure in MARS-5 ensures complete decomposition of BHVO-2, BCR-2, UB-N followed by ICP-MS determination of 32 specified elements in the obtained solutions without additional preconcentration steps. The relative standard deviations for the determined elements are 2 – 9% for the reference materials BHVO-2, BCR-2, 3 – 12% for UB-N with an increase to 16 – 25% (Nb, Ta) due to the approach to the detection limit. The more efficient microwave digestion in UltraWAVE compared to MARS-5 was proved by the complete decomposition of JP-1 with the transfer of all the elements, including Cr, to the solution.

Water Degradation in ITER Neutral Beam Test Facility Cooling Circuits

Source for production of ion of deuterium extracted from rf plasma (SPIDER) is the 100 keV negative ion source prototype of the ITER neutral beam injector. The cooling plant is one of the SPIDER auxiliary systems where ultrapure water (UPW) is used as the cooling media, thanks to its advantageous properties such as good cooling performance and high resistivity. Water resistivity needs to be maintained above certain values during SPIDER operation to enable the electrical insulation of in-vessel components that operate at different voltages. Nonetheless, degradation of water resistivity was observed in some circuits during operation. Water resistivity degradation had a negative impact on the SPIDER experimental campaign since it limits cooling plant availability. To understand the cause for the observed water degradation, sampling points were installed to sample water during operation. Ad hoc experiments have been performed on the worst affected circuit, and water samples were analyzed by inductively coupled plasma mass spectrometry (ICP-MS). Circulation experiments were conducted at constant temperature, pressure, and flow rate to assess water degradation by monitoring water conductivity increase. ICP-MS analyses on water from the worst affected circuit revealed the presence of Cu in relevant quantities and Zn. Corrosion induced by the presence of a non-compatible component with SPIDER requirements was found. The identified component was made of a galvanized steel plate, carbon steel, and brass. This was found responsible for the contamination of the cooling loop and its water properties’ degradation.

The influence of H2 partial pressure on biogenic palladium nanoparticle production assessed by single-cell ICP-mass spectrometry.

The production of biogenic palladium nanoparticles (bio-Pd NPs) is widely studied due to their high catalytic activity, which depends on the size of nanoparticles (NPs). Smaller NPs (here defined as <100 nm) are more efficient due to their higher surface/volume ratio. In this work, inductively coupled plasma-mass spectrometry (ICP-MS), flow cytometry (FCM) and transmission electron microscopy (TEM) were combined to obtain insight into the formation of these bio-Pd NPs. The precipitation of bio-Pd NPs was evaluated on a cell-per-cell basis using single-cell ICP-MS (SC-ICP-MS) combined with TEM images to assess how homogenously the particles were distributed over the cells. The results provided by SC-ICP-MS were consistent with those provided by "bulk" ICP-MS analysis and FCM. It was observed that heterogeneity in the distribution of palladium over an entire cell population is strongly dependent on the Pd2+ concentration, biomass and partial H2 pressure. The latter three parameters affected the particle size, ranging from 15.6 to 560 nm, and exerted a significant impact on the production of the bio-Pd NPs. The TEM combined with SC-ICP-MS revealed that the mass distribution for bacteria with high Pd content (144 fg Pd cell-1 ) indicated the presence of a large number of very small NPs (D50=15.6nm). These results were obtained at high cell density (1 × 105 ± 3 × 104 cells μl-1 ) and H2 partial pressure (180 ml H2 ). In contrast, very large particles (D50=560 nm) were observed at low cell density (3 × 104 ± 10 × 102 cells μl-1 ) and H2 partial pressure (10-100 ml H2 ). The influence of the H2 partial pressure on the nanoparticle size and the possibility of size-tuned nanoparticles are presented.

Development and application of an analysis method for the determination of rare earth elements in silicate-rich samples by Na2O2 sintering and ICP-MS analysis.

The performance of a fast and simple analytical procedure for rare earth elements (REEs) quantification from secondary sources was investigated in the present work. Seven silicate-rich certified reference materials (CRMs) in the form of Andesite (JA-1), Basalt (JB-3), Rhyolite (JR-1, JR-2), Granite (JG-2), Granodiorite (JG-3), and Till (TILL-1), were used for the optimization and characterization of the analysis method. The optimized method was used in the analysis of nine mining wastes selected within the ENVIREE project, under the ERA-MIN Program of the 7th Framework, having as the main aim to ensure a policy securing long-term access of REEs secondary sources at reasonable costs. For silicate-rich samples efficient solid dissolution involves sintering with Na2O2 at 460°C and a sample to oxidizing reagent ratio of 1:6.5. Inductively coupled plasma-mass spectrometry (ICP-MS) was used in the quantification of the REEs with aerosol dilution of samples applied to minimize the salt effect on the plasma and interface regions. The work performed in the present study clearly shows that accurate reports on the REE concentrations from geological matrices also involves as mandatory the estimation of the overall uncertainty from various sources (sample preparation or analyte measurements). In the analysis of geological samples, the proposed analysis method has on average 23% of the overall uncertainty explained by the sample preparation and 77% accounted by the analysis steps. Moreover, the method described by effective, cheap, robust and safe attributes, can be recommended as an accessible alternative to the HF wet digestion method. Although from all the investigated tailings samples, only those from Sweden and Czech Republic can be regarded as potential secondary sources for REEs, investigation of other resources with interest at European level might bring a great benefit in the general attempt to develop an economically viable method for the production of rare earth elements.

Feasibility of direct analysis of algae contamination with chromium and copper on the filter with laser-induced breakdown spectroscopy and laser ablation inductively coupled plasma mass spectrometry

The chromium and copper contamination of algae on a filter was directly monitored with laser-induced breakdown spectroscopy (LIBS) as a demonstration of LIBS capabilities. Liquid samples of the green alga Desmodesmus subspicatus were intentionally contaminated with chromium, incubated, filtered, and the filters with the algae were analysed. Inductively coupled plasma mass spectrometry (ICP-MS) was used as a reference method. One half of the filter with the algae was dissolved and analysed as a solution with ICP-MS and the second half was subjected to the LIBS and laser ablation-ICP-MS analysis. Chromium and copper were attributable to the algae contamination and detectable with LIBS. The results from the LIBS provided almost equivalent information about the relative changes of the Cr and Cu concentration in the algae. The sensitivity of LIBS with a Czerny-Turner spectrometer was fully comparable with the ICP-MS procedure. The trends from LIBS were more similar to the LA-ICP-MS ones. It means that the algae growth inhibition in dependence on the chromium or copper content can be alternatively monitored with LIBS instead of the complicated decomposition procedure in ICP-MS analysis.

Titanium wear from magnetically controlled growing rods (MCGRs) for the treatment of spinal deformities in children

Magnetically controlled growing rods (MCGRs) are an effective treatment method for early-onset scoliosis (EOS). In recent years, increasing titanium wear was observed in tissue adjacent to implants and in blood samples of these patients. This study aims to investigate the potential correlation between amount of metal loss and titanium levels in blood during MCGR treatment as well as influencing factors for metal wear. In total, 44 MCGRs (n = 23 patients) were retrieved after an average of 2.6 years of implantation and analyzed using a tactile measurement instrument and subsequent metal loss calculation. Titanium plasma levels (n = 23) were obtained using inductively coupled plasma-mass spectrometry (ICP-MS). The correlation of both parameters as well as influencing factors were analyzed. Titanium abrasion on MCGRs was observed in the majority of implants. There was no correlation of metal implant wear or titanium plasma values to the duration of MCGR implantation time, number of external lengthening procedures, patient’s ambulatory status, gender, weight or height. Material loss on the MCGRs showed a positive correlation to titanium blood plasma values. The present study is one of the first studies to analyze retrieved MCGRs using high-precision metrological techniques and compare these results with ICP-MS analyses determining blood titanium values.

Competitive Interactions Between Microbial Siderophores and Humic-Like Binding Sites in European Shelf Sea Waters

Siderophores are low molecular weight high affinity iron chelates found at low concentrations in seawater. In this study we determined the total concentrations and identities of siderophores in extracts isolated from a shelf sea environment on the Northwest European shelf by high performance liquid chromatography coupled to high resolution inductively coupled plasma mass spectrometry (ICP-MS) in parallel to high resolution electrospray ionisation mass spectrometry (ESI-MS). We identified a total of 24 different siderophores in our samples via metal isotope profiling of masses detected by ESI-MS. Twenty three of the identified siderophores could be assigned to three siderophore families – ferrioxamines, amphibactins and marinobactins. In contrast, only 12 peaks could be resolved in iron chromatograms obtained via ICP-MS analysis. Comparison of results obtained by the two mass spectrometry detectors showed that neither method was able to detect and identify all siderophores present in the samples on its own. We assessed the impact of our observed total siderophore concentrations on iron speciation by calculating the distribution of iron species as a function of total siderophore concentrations at different iron concentrations representative of our study area. We considered competition for iron between siderophores, a humic like dissolved organic matter (DOM) fraction and hydroxide ions by combining an ion-pair model with a non-ideal competitive interaction (NICA)-Donnan model. We found that the overall impact of siderophores on iron biogeochemistry is low at concentrations of siderophore &amp;lt;100 pmol L-1, and that the dominant iron species present at siderophore concentrations of the order of a few tens of pmol L-1 will be iron bound to the humic like DOM fraction. Furthermore the heterogeneity of binding sites in the humic like DOM fraction means that other binding sites present in organic matter could be effective competitors for siderophores, especially at low iron concentrations. Our findings highlight the importance of binding site heterogeneity when considering the influence of different iron binding groups on iron speciation in the marine environment.

Assessment of geographical origin of virgin coconut oil using inductively coupled plasma mass spectrometry along with multivariate chemometrics

Recently, Virgin coconut oil (VCO) has emerged as one of the most favorable edible oils because of its application in cooking, frying as well as additive used in food, pharmaceuticals, and cosmetic goods. These qualities have established VCO in high consumer demand and there is a great need of establishing a reliable method for the identification of its geographical origin. Through this present study, for the first time, it has been established that Inductively Coupled Plasma-Mass-Spectrometry (ICP-MS) combined with multivariate chemometrics can be used for the identification of the geographical origin of the VCO samples of various provinces. Principal Component Analysis (PCA), and Linear Discriminant Analysis (LDA) were able to differentiate and classify the VCO samples of different geographical origins. Further, calibration models (Principal Component Regression and Partial Least Square Regression) were developed on the calibration dataset of the elemental concentration obtained from the ICP-MS analysis. An external dataset was used to develop the prediction model to predict the geographical origin of an unknown sample. Both PCR and PLS-R models were successfully able to predict the geographical origin with a high R2 value (0.999) and low RMSEP value 0.074 and 0.075% v/v of prediction respectively. In conclusion, ICP-MS combined with regression modelling can be used as an excellent tool for the identification of the geographical origin of the VCO samples of various provinces. This whole technique is the most suitable as it has high sensitivity as well as provides easy multi-metal analysis for a single sample of edible oil.

Effects of route of administration on neural exposure to platinum-based chemotherapy treatment: a pharmacokinetic study in rat

The persisting need for effective clinical treatment of chemotherapy-induced neurotoxicity (CIN) motivates critical evaluation of preclinical models of CIN for their translational relevance. The present study aimed to provide the first quantitative evaluation of neural tissue exposed in vivo to a platinum-based anticancer compound, oxaliplatin (OX) during and after two commonly used dosing regimens: slow IV infusion used clinically and bolus IP injection used preclinically. Inductively-coupled plasma mass spectrometry analysis of dorsal root ganglia indicated that while differences in the temporal dynamics of platinum distribution exist, key drivers of neurotoxicity, e.g. peak concentrations and exposure, were not different across the two routes of administration. We conclude that the IP route of OX administration achieves clinically relevant pharmacokinetic exposure of neural tissues in a rodent model of CIN.

Synthesis and Characterization of Poly(pyrrole-1-carboxylic acid) for Preconcentration and Determination of Rare Earth Elements and Heavy Metals in Water Matrices.

Pyrrole was N-functionalized with solid carbon dioxide followed by chemical polymerization to create a new air-stable, granular, and water-insoluble sorbent, poly(pyrrole-1-carboxylic acid) (PPy-CO2). PPy-CO2 exhibited enhanced affinity for the sorption of metal ions compared to unfunctionalized PPy due to the incorporation of carboxylate functional groups directly onto the polymer backbone. As a freestanding sorbent material, immobilization to an additional solid support is not needed. Sorption, and therefore preconcentration, occurs simultaneously to achieve efficient removal and recovery of metal ions by a pH-dependent sorption-desorption mechanism. PPy-CO2 was evaluated on the analytical scale for the solid-phase extraction of a range of metal ions and found to efficiently preconcentrate rare earth elements (REEs), Th, and heavy metals (Cr, Fe, Cd, and Pb), which allowed quantitation by inductively coupled plasma mass spectrometry (ICP-MS). The impact of sorption parameters, such as solution pH, amount of sorbent, and sorption time, and the effect of desorption flow rate for recovery were investigated and optimized using ultrasound-assisted dispersive solid-phase extraction (UAD-SPE) with ICP-MS analysis. Maximum efficiency for sorption and recovery of most metal ions was achieved at a solution pH of 6.0, 10 mg of sorbent, a sorption time of 5 min, and desorption conditions of 1 mL of 2 M nitric acid applied at a flow rate of 0.25 mL min-1. Detection limits for REEs and Th ranged from 0.2-3.4 ng L-1 for REEs and Th and 0.9-5.7 ng L-1 for heavy metals. Linear ranges from 0.1-1000 μg L-1 for REEs and 0.1-500 μg L-1 for heavy metals and Th were also observed. PPy-CO2 successfully preconcentrated and facilitated the determination of the targeted metal ions in water matrices of varying complexity, including tap water, well water, river water, and produced water samples. These results indicate the potential application of PPy-CO2 for larger-scale recovery and removal of valuable or hazardous metal ions.

Modified amino-dextrans as carriers of Gd-chelates for retrograde transport and visualization of peripheral nerves by magnetic resonance imaging (MRI)

Amino-dextrans (AD) conjugated with gadolinium (Gd3+) were developed as neuro-specific contrast agents (CA) for the visualization of the sciatic nerve in rats by magnetic resonance imaging (MRI). AD with 3, 10, and 70 kDa molecular weights were assessed as carrier molecules known to be transported with various speed by axonal microtubules. Detailed spectroscopic characterizations, analyses by Fast Protein Liquid Chromatography (FPLC), Sodium Dodecyl Sulfate Polyacrylamide Gel Electrophoresis (SDS-PAGE), and inductively coupled plasma-mass spectrometry (ICP-MS), were carried out. For MRI, the paramagnetic Gd3+ ion was coupled as a T1 signal enhancer. The well-established linear chelator, diethylenetriaminepentaacetic acid (DTPA), was used and subsequently replaced by the more stable cyclic chelator 1,4,7,10-Tetraazacyclododecane-1,4,7,10-tetraacetic acid (DOTA). In addition, a fluorescently labeled AD-DTPA-Gd was prepared to demonstrate an active transport to the spinal cord by histochemistry. After successful synthesis and characterization, molecular migration of the AD-DTPA-Gd in the sciatic nerve of healthy Sprague Dawley rats was monitored by MRI for up to seven days. Enhancement of nerve structures was evaluated by MRI and correlated with ICP-MS analyses. To investigate the distribution of CA along the neuraxis, all animals were sacrificed after the final MRI monitoring. Nerves, spinal ganglions, and corresponding spinal cord sections were harvested, to determine the localization and concentration of the paramagnetic element. This is the first report that demonstrates the active uptake and transport of AD-Gd conjugates within the sciatic nerve. This new concept may serve as a potential diagnostic tool for the direct visualization and monitoring of the continuity of injured nerves.

The assessment of effectiveness of SEM- EDX and ICP-MS methods in the process of determining the mineralogical and geochemical composition of particulate matter deposited on spider webs

Air pollution can be monitored using many different methods. In this paper, we aimed to test and validate two analytical techniques based on complex mineralogical and geochemical analyses with the use of spider webs as a passive sampler. The samples of spider webs were collected in 2018 in polluted areas in the vicinity of the copper smelter Głogów (Poland). Samples were analysed using scanning electron microscopy with energy dispersive x-ray analysis (SEM-EDX) to obtain not only the information about the form and size of studied particles but also their origin (anthropogenic or terrigenous). Geochemical analysis was performed using inductively coupled plasma mass spectrometry (ICP-MS), providing the total amount of chosen and potentially toxic elements. The frequency of metal occurrence in atmospheric particles identified with the use of SEM-EDX was compared with the results from ICP-MS and recalculated into the percentage of contribution. A significant correlation between chemical and mineralogical composition was found demonstrating that the phases and minerals were correctly recognised and properly divided into groups. For elements such as Pb, Zn, and Cu, which are the major contaminants in the study area, the validation of the method gave good results, revealing the convergence of results for most sampling points. Finally, our study showed that the results obtained by SEM-EDX analysis can be comparable to quantitative results (ICP-MS analysis).

Self-templated hollow nanospheres of B-site engineered non-stoichiometric perovskite for supercapacitive energy storage via anion-intercalation mechanism

The continual increase in energy demand and inconsistent supply have attracted attention towards sustainable energy storage/conversion devices, such as electrochemical capacitors with high energy densities and power densities. Perovskite oxides have received significant attention as anion-intercalation electrode materials for electrochemical capacitors. In this study, hollow nanospheres of non-stoichiometric cubic perovskite fluorides, KNi1−xCoxF3−δ (x = 0.2; δ = 0.33) (KNCF-0.2) have been synthesized using a localized Ostwald ripening. The electrochemical performance of the non-stoichiometric perovskite has been studied in an aqueous 3 M KOH electrolyte to categorically investigate the fluorine-vacancy-mediated charge storage capabilities. High capacities up to 198.55 mA h g−1 or 714.8 C g−1 (equivalent to 1435 F g−1) have been obtained through oxygen anion-intercalation mechanism (peroxide pathway, O-). The results have been validated using ICP (inductively coupled plasma mass spectrometry) analysis and cyclic voltammetry. An asymmetric supercapacitor device has been fabricated by coupling KNCF-0.2 with activated carbon to deliver a high energy density of 40 W h kg−1 as well as excellent cycling stability of 98% for 10,000 cycles. The special attributes of hollow-spherical, non-stoichiometric perovskite (KNCF-0.2) have exhibited immense promise for their usability as anion-intercalation type electrodes in supercapacitors.