Inductively Coupled Plasma Mass Spectrometry Analysis Research Articles

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.

Observation of targeted gold nanoparticles in nasopharyngeal tumour nude mice model through dual-energy computed tomography.

This study was performed to specify the efficiency of imaging nanoparticle concentration as contrast media in dual‐energy computed tomography (DECT). Gold nanoparticles (AuNPs) and gold nanoparticles‐conjugated folic acid through cysteamine (FA‐Cya‐AuNPs) were both considered as contrast agents. Characterization of NPs was performed using Dynamic Light Scattering (DLS) and zeta potential. The hemocompatibility of NPs was confirmed by different blood parameters such as white blood cell, red cell distribution width, hemoglobin, lymphocytes counts and haemolysis assay. DECT algorithm was confirmed using calibration phantom at different concentrations of NPs and tube potentials (80 and 140 kVp). Then, DECT was used to quantify the concentration of both AuNPs and FA‐Cys‐AuNPs in human nasopharyngeal cancer cells. Mice were injected with non‐targeted AuNPs and targeted AuNps at a concentration of 3 × 103 μg/ml. Then, they were scanned with different tube potentials. The concentration of nanoparticles in the various organs of nude mice was measured through DECT imaging and inductively coupled plasma mass spectrometry (ICP‐MS) analysis. The results of DECT images were compared with ICP‐MS analysis and indicated that they were approximately similar. In sum, FA‐Cys‐AuNPs can be a proper candidate for targeted contrast media in DECT molecular scanning of human nasopharyngeal tumours.

Nanographene oxide modified phenyl methanethiol nanomagnetic composite for rapid separation of aluminum in wastewaters, foods, and vegetable samples by microwave dispersive magnetic micro solid-phase extraction

A new method based on graphene oxide modified (4-phenyl) methanethiol nanomagnetic composite (Fe3O4@4-PhMT-GO) was used for extraction and separation of aluminum from wastewater, food, and vegetable samples in aluminum cookware by microwave dispersive magnetic micro solid-phase extraction (MDM-μ-SPE). In optimized conditions, the working range (WR), the linear range (LR), the limit of detection (LOD), and enrichment factor (EF) were obtained 5–5200 μg L−1, 5–1600 μg L−1, 1.5 µg L−1, and 48.8, respectively (RSD% = 2.5). By MDM-μ-SPE procedure, the aluminum concentrations in baking rice and spinach with aluminum cookware were obtained 97.43 ± 2.57 mg g−1 and 131.64 ± 5.18 mg g−1, respectively which was analyzed by atom trap flame atomic absorption spectrometer (AT-FAAS). The results showed, the aluminum concentrations in cooked foods with Teflon cookware were less than aluminum cookware. The methodology was validated by standard reference materials (SRM) and inductively coupled plasma mass spectrometry analysis (ICP-MS).

Investigation on Dissolution and Removal of Adhered LiCl-KCl-UCl<sub>3</sub> Salt From Electrodeposited Uranium Dendrites using Deionized Water, Methanol, and Ethanol

Deionized water, methanol, and ethanol were investigated for their effectiveness at dissolving LiCl-KCl-UCl3 at 25, 35, and 50℃ using inductively coupled plasma mass spectrometry (ICP-MS) to study the concentration evolution of uranium and mass ratio evolutions of lithium and potassium in these solvents. A visualization experiment of the dissolution of the ternary salt in solvents was performed at 25℃ for 2 min to gain further understanding of the reactions. Aforementioned solvents were evaluated for their performance on removing the adhered ternary salt from uranium dendrites that were electrochemically separated in a molten LiCl-KCl-UCl3 electrolyte (500℃) using scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS). Findings indicate that deionized water is best suited for dissolving the ternary salt and removing adhered salt from electrodeposits. The maximum uranium concentrations detected in deionized water, methanol, and ethanol for the different temperature conditions were 8.33, 5.67, 2.79 μg·L-1 for 25℃, 10.62, 5.73, 2.50 μg·L-1 for 35℃, and 11.55, 6.75, and 4.73 μg·L-1 for 50℃. ICP-MS analysis indicates that ethanol did not take up any KCl during dissolutions investigated. SEM-EDS analysis of ethanol washed uranium dendrites confirmed that KCl was still adhered to the surface. Saturation criteria is also proposed and utilized to approximate the state of saturation of the solvents used in the dissolution trials.

Detection of U-87 Tumor Cells by RGD-Functionalized/Gd-Containing Giant Unilamellar Vesicles in Magnetization Transfer Contrast Magnetic Resonance Images.

The targeting of tumor cells and their visualization with magnetic resonance imaging (MRI) is an important task in biomedicine. The low sensitivity of this technique is a significant drawback and one that may hamper the detection of the imaging reporters used.To overcome this sensitivity issue, this work explores the synergy between 2 strategies: (1) arginine, glycine, aspartic acid peptide (RGD)-functionalized giant unilamellar vesicles (GUVs) loaded with Gd complexes to accumulate large amounts of MRI contrast agent at the targeting site; and (2) the use of magnetization transfer contrast (MTC), which is a sensitive MRI technique for the detection of Gd complexes in the tumor region. Giant unilamellar vesicles were prepared using the gentle swelling method, and the cyclic RGD targeting moiety was introduced onto the external membrane. Paramagnetic Gd-containing complexes and the fluorescent probe rhodamine were both part of the vesicle membranes and Gd-complexes were also the payload within the inner aqueous cavity. Giant unilamellar vesicles that were loaded with the imaging reporters, but devoid of the RGD targeting moiety, were used as controls. U-87 MG human glioblastoma cells, which are known to overexpress the targets for RGD moieties, were used. In the in vivo experiments, U-87 MG cells were subcutaneously injected into nu/nu mice, and the generated tumors were imaged using MRI, 15 days after cell administration. Magnetic resonance imaging was carried out at 7 T, and T2W, T1W, and MTC/Z-spectra were acquired. Confocal microscopy images and Inductively Coupled Plasma Mass Spectrometry (ICP-MS) were used for result validation. In vitro results show that RGD GUVs specifically bind to U-87 MG cells. Microscopy demonstrates that (1) RGD GUVs were anchored onto the external surface of the tumor cells without any internalization; (2) a low number of GUVs per cell were clustered at specific regions; and (3) there is no evidence for macrophage uptake or cell toxicity. The MRI of cell pellets after incubation with RGD GUVs and untargeted ctrl-GUVs was performed. No difference in T1 signal was detected, whereas a 15% difference in MT contrast is present between the RGD GUV-treated cells and the ctrl-GUV-treated cells.Magnetic resonance imaging scans of tumor-bearing mice were acquired before and after (t = 0, 4 hours and 24 hours) the administration of RGD GUVs and ctrl-GUVs. A roughly 16% MTC difference between the 2 groups was observed after 4 hours. Immunofluorescence analyses and ICP-MS analyses (for Gd-detection) of the explanted tumors confirmed the specific accumulation of RGD GUVs in the tumor region. RGD GUVs seem to be interesting carriers that can facilitate the specific accumulation of MRI contrast agents at the tumor region. However, the concentration achieved is still below the threshold needed for T1w-MRI visualization. Conversely, MTC proved to be sufficiently sensitive for the visualization of detectable contrast between pretargeting and posttargeting images.

Basal Ti level in the human placenta and meconium and evidence of a materno-foetal transfer of food-grade TiO2 nanoparticles in an ex vivo placental perfusion model

BackgroundTitanium dioxide (TiO2) is broadly used in common consumer goods, including as a food additive (E171 in Europe) for colouring and opacifying properties. The E171 additive contains TiO2 nanoparticles (NPs), part of them being absorbed in the intestine and accumulated in several systemic organs. Exposure to TiO2-NPs in rodents during pregnancy resulted in alteration of placental functions and a materno-foetal transfer of NPs, both with toxic effects on the foetus. However, no human data are available for pregnant women exposed to food-grade TiO2-NPs and their potential transfer to the foetus. In this study, human placentae collected at term from normal pregnancies and meconium (the first stool of newborns) from unpaired mothers/children were analysed using inductively coupled plasma mass spectrometry (ICP-MS) and scanning transmission electron microscopy (STEM) coupled to energy-dispersive X-ray (EDX) spectroscopy for their titanium (Ti) contents and for analysis of TiO2 particle deposition, respectively. Using an ex vivo placenta perfusion model, we also assessed the transplacental passage of food-grade TiO2 particles.ResultsBy ICP-MS analysis, we evidenced the presence of Ti in all placentae (basal level ranging from 0.01 to 0.48 mg/kg of tissue) and in 50% of the meconium samples (0.02–1.50 mg/kg), suggesting a materno-foetal passage of Ti. STEM-EDX observation of the placental tissues confirmed the presence of TiO2-NPs in addition to iron (Fe), tin (Sn), aluminium (Al) and silicon (Si) as mixed or isolated particle deposits. TiO2 particles, as well as Si, Al, Fe and zinc (Zn) particles were also recovered in the meconium. In placenta perfusion experiments, confocal imaging and SEM-EDX analysis of foetal exudate confirmed a low transfer of food-grade TiO2 particles to the foetal side, which was barely quantifiable by ICP-MS. Diameter measurements showed that 70 to 100% of the TiO2 particles recovered in the foetal exudate were nanosized.ConclusionsAltogether, these results show a materno-foetal transfer of TiO2 particles during pregnancy, with food-grade TiO2 as a potential source for foetal exposure to NPs. These data emphasize the need for risk assessment of chronic exposure to TiO2-NPs during pregnancy.

Determination of Metals in Tree Rings by ICP-MS Using Ash from a Direct Mercury Analyzer

Elemental profiles in cores of tree trunks (bole wood) have been used for environmental monitoring and reconstruction of metal pollution history. Mercury (Hg) is a global pollutant that can be accurately measured in tree rings in a simple and pragmatic fashion using a direct mercury analyzer (DMA) that is based on thermal decomposition, amalgamation, and atomic absorption spectrophotometry. In this feasibility study, we demonstrate that the ash remaining after the DMA analyses can be used to quantify a wide range of other non-volatile elements (Ba, Be, Co, Cr, Cu, Fe, Ga, Mg, Mn, Ni, Pb, Sr, Th, and U) in that same sample of wood by inductively coupled plasma mass spectrometry (ICP-MS) after microwave-assisted acid digestion. Other elements (Ag, Cd, Cs, Rb, Tl, and V) exhibited poor recoveries, possibly due to losses during sample preparation. We assessed the accuracy with reference materials, spikes, and by comparison with EPA Method 3052 (Microwave Assisted Acid Digestion of Siliceous and Organically Based Matrices). For the first group of elements (deemed suitable for the method), recoveries ranged between 80% and 120% and the relative standard deviation was generally < 15%, indicating acceptable precision. We applied the method to five species of trees: eastern red cedar (Juniperus virginiana), loblolly pine (Pinus taeda), shortleaf pine (Pinus echinata), white oak (Quercus alba), and tulip poplar (Liriodendron tulipifera) from Holly Springs National Forest in north Mississippi, USA. Mercury concentrations (ng/g ± SE) were highest in the cedar (1.8 ± 0.3; n = 5), followed by loblolly pine (1.6 ± 0.3, n = 3), shortleaf pine (1.2 ± 0.2; n = 3), oak (1.1 ± 0.2; n = 5), and poplar (0.5 ± 0.1; n = 5). Concentrations of other elements were generally Fe > Mg > Ba ≈ Sr ≈ Mn > Cr ≈ Cu > Ni ≈ Rb > Co > Ga ≈ Ag, with the other elements generally below the method detection limit (MDL). Overall, we showed that the DMA can be used to not only determine total Hg in segments of tree core, but can serve as the ashing step in the preparation of wood for ICP-MS analysis, thus allowing the determination of non-volatile elements along with Hg in the very same sample.

Characterization of Cabernet Sauvignon wines from California: determination of origin based on ICP-MS analysis and machine learning techniques

In this paper, samples of Cabernet Sauvignon wines produced in California have been analyzed on the basis of their elemental content and classified according to its geographical origin by the use of machine learning. Overall, 13 metals (Al, Cd, Co, Cr, Cu, Li, Mn, Ni, P, Pb, Rb, Sr, and Zn) were determined by inductively coupled plasma mass spectrometry (ICP-MS). We used two algorithms of variable selection in order to estimate the relevance of each metal to classification. Predictive models based on chemometric tools and machine learning algorithms were developed to differentiate origin of wine samples. Li and Sr were identified as the main responsible for the differentiation of samples. The application of Random Forest permitted to correctly classify all samples. A second analysis was performed by removing the variables Li and Sr to investigate the relevance of the others metals. We found that a group of seven variables (Cd, Ni, Mn, Pb, Rb, Co, Cu) which were able to discriminate the wines in 89% of accuracy by using Support Vector Machines. Results suggested that the developed methodology by advanced machine learning techniques is robust and reliable for the geographical classification of wine samples, and the study of the elements that characterize the regions.

Feasibility of microwave-induced combustion combined with inductively coupled plasma mass spectrometry for bromine and iodine determination in human nail.

Bromine and iodine have important physiological functions; however, in inadequate concentration, they can also cause several physiological problems. Their mobility assessment in human organisms through biological sampling may help clarify some doubts related to metabolic routes, which are still not well elucidated. In this context, a suitable analytical method for this purpose should be developed. An analytical method for determining ultratrace levels of bromine and iodine in human nail samples was developed. Inductively coupled plasma mass spectrometry (ICP-MS) using a conventional nebulization system was immediately chosen as the determination tool because of its powerful sensitivity and selectivity. Sample preparation methods including microwave-induced combustion (MIC), microwave-assisted extraction, and microwave-assisted digestion were evaluated. The compatibility of the final solutions with ICP-MS analysis was considered while the method was developed. MIC was chosen as the most suitable method for the sample preparation for determining the levels of bromine and iodine in human nail samples using ICP-MS. Unlike other sample preparation methods, this one fully eliminated interferences related to the carbon content and memory effects. Sample masses up to 100 mg were efficiently digested, and the analytes were quantitatively absorbed using only 50 mmol L-1 NH4 OH solution. Recoveries ranged from 93% to 102%, and the relative standard deviation was < 8%. The proposed analytical method presents important characteristics for routine analysis. It allows ultratrace determination even when low sample masses are used because of the low blank values, reduced volume of reagents, and powerful detectability using ICP-MS.

Thallium toxicity due to audultered infusion with thallium sulfate in eight members belonging to the same family nucleus: Autopsy findings and ICP-MS analysis (inductively coupled plasma mass spectrometry) in a triple homicide.

The banning of the heavy metal thallium (Tl) in many Countries, because of its toxicity, led to a remarkable reduction of the number of cases of poisoning both accidental and homicidal forcing us to better study the pharmacokinetics of this poison using new technologies. The Authors, in this work, are reporting the case of a collective thallium toxicosis caused by voluntary adulteration of an infusion with thallium sulfate, occurred in 8 members of the same familial nucleus; the administration of Prussian Blu resulted to be ineffective for 3 of these members that died at a later time. The most peculiar aspects of this rare manner of poisoning are discussed; the analytical procedures used, Inductively Coupled Plasma Mass Spectrometry (ICP-MS) in particular, resulted to be fundamental in the forensic diagnosis process of acute poisoning cause by thallium.

Investigation of structural-geometric parameters and elemental composition of spherical VT20 alloy powders

Purpose: Identification of structural-geometrical parameters, technological properties and elemental composition of spherical powders in a wide fraction range with respect to the VT20 alloy has been carried out. This is important for evaluating the optimum filling of a given volume by mixture of powders of different fractions during 3D printing. Design/methodology/approach: During the investigation of spherical Ti-alloy powders, a comprehensive approach was performed using Scanning Electron Microscopy (SEM), Energy-Dispersive X-ray Spectroscopy (EDS), Dynamic Light Scattering (DLS) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). The surface morphology of the powders was studied on a Tuescan Vega 3 Scanning Electron Microscope. Using the Quantax energy dispersive spectrometer, element distribution maps were obtained and histograms of element distribution in the investigated powders were constructed. ICP-MS analysis was performed to clarify the elemental composition. DLS analysis using Malvern's Zetasizer Nano-ZS equipment allowed us to determine the functional parameters (hydrodynamic radius – Rh, zeta potential – z and specific conductivity) of particles of titanium alloy powder that indirectly indicate a tendency to form conglomerates. Findings: According to the microscopic examinations, the VT20 alloy powder consists of globular-shaped particles with the lamellar traces on their surfaces. The uniformity of the chemical element distribution within each fraction of the investigated powders was confirmed by EDS, and the full conformity of the powder fractions with the elemental composition of the VT20 alloy was confirmed by ICP-MS. The DLS method allowed to establish that the formation of conglomerates would not occur within the studied fractions of the VT20 alloy powder. Research limitations/implications: The use of high sensitive investigation methods gives understanding of the mechanisms of fine structure formation and possibility to control the processes of powder coagulation in the stage of electrostatic interactions. Practical implications: The obtained results can be used for the formation of fine spherical particles of the powder, but at the same time, these technologies can be extended for the particles of non-spherical shape. Originality/value: The DLS method allowed to establish that the formation of conglomerates would not occur within the studied fractions of the VT20 alloy powder. This, in turn, will improve powder melting during 3D printing. The measured zeta potential values allowed us to reveal mechanisms of fine structure formation and to control the processes of powder coagulation in the stage of electrostatic interactions.

Sulfur-free Surfactant for Carbide Nanoparticle Characterization in Steel Using Asymmetric Flow Field-Flow Fractionation Hyphenated Inductively Coupled Plasma-Mass Spectrometry.

An asymmetric flow field-flow fractionation (AF4) combined with inductively coupled plasma mass spectrometry (ICP-MS) was applied to measure the concentration and size distribution of nanometer-sized carbides in steel sheets, such as titanium carbides (TiC) and vanadium carbides (VC). Prior to AF4-ICP-MS measurement, TiC and VC nanoparticles in steel were extracted into a solution via selective potentio-static etching by electrolytic dissolution (SPEED) method. The SPEED method enabled the selective dissolution of iron and the carbide nanoparticles were dispersed as primary particles in solution with surfactant. However, sulfur-free surfactant was required in AF4-ICP-MS carrier solutions because sulfur in SDS, generally used to disperse various nanoparticles, causes a spectral interference with titanium and vanadium in ICP-MS analysis. In this study, sulfur-free sodium cholate (SC) was applied as the dispersant of carbide nanoparticles for the SPEED method and AF4 measurements. SC provides a high absolute value of zeta potential on a particle surface and membrane of an AF4 separation channel to prevent particle adsorption on the membrane. Additionally, SC does not generate the spectral interference due to sulfur, in contrast to SDS. Thus, it enabled the sensitive detection of titanium and vanadium in carbide nanoparticles extracted from a steel sheet in AF4-ICP-MS. These results indicate that sulfur-free surfactants are useful for analyzing some precipitates in steels using AF4-ICP-MS.

Inductively coupled plasma mass spectrometry assay for quantification of free infliximab in serum

TNF antagonists such as infliximab are effective for the treatment of several inflammatory and autoimmune diseases. Recent clinical studies have advocated the importance of measuring trough infliximab levels to guide treatment decisions. We have developed a novel assay for measuring serum free infliximab levels using inductively coupled plasma-mass spectrometry (ICP-MS). The method involves the incubation of patient serum in wells coated with recombinant TNF, followed by detection with lanthanide-labeled monoclonal anti-human IgG1 and ICP-MS analysis. Full method validation was performed and results for clinical samples tested with the new method were compared with those obtained from a capture ELISA and a cell-based assay. Validation of the ICP-MS assay revealed a lower limit of detection of 0.4 μg/mL in serum. The linear range of quantitation was 1–50 μg/mL. The within-run and between-run precision had a coefficient of variation (CV) of <10%, and the accuracy of the assay had a CV of <15%. In serum samples, the ICP-MS method was devoid of analytical interferences by high levels of hemoglobin, bilirubin and triglycerides. Serum sample results from 123 drug-naïve donors revealed a test cutoff at 0.5 μg/mL. Test results from clinical samples obtained by the ICP-MS method showed strong correlation with both the ELISA and cell-based assay. The ICP-MS methodology presented in this study is a robust method for measuring TNF antagonist serum levels, which makes it well suited for therapeutic drug monitoring in the clinical laboratory.

Exploratory and comparative analysis of the morphology and chemical composition of PM2.5 from regions with different socioeconomic characteristics

Chemical and physical properties of fine particulate matter (PM2.5) are related to emission sources. In order to determine chemical and physical differences, PM2.5 samples were collected at urban, rural and industrial areas of the metropolitan region of Rio de Janeiro (MRRJ), Brazil. The chemical characterization of the samples was performed using ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP-MS), while the physical characterization was done by scanning electron microscopy–energy dispersive spectrometry (SEM-EDS). Through the use the Hybrid Single-Particle Lagrangian Integrated Trajectories (HYSPLIT) model, it was observed that all the studied sites presented the influence of ocean air masses. The industrial and rural sites showed to influence of continental air masses too, that carried aerosols with greater UV absorption compared to those observed in trajectories originating in the Atlantic Ocean. Among analyzed species, NO3− and SO42− ions and V, Pb and Sn elements were predominant in the urban site whereas in the rural and industrial sites Na+, SO42− were the major ions and Na, Zn and Ba were the elements with the higher concentrations. Through SEM-EDS analysis, the particles were classified into two categories, the first in terms of the morphological similarities and the second in function of the elemental composition. As observed in ICP-MS analysis, the elements K, Al, Ca, Fe, Cu, Zn, Ba and Mg were detected also in the individual particles analysis by SEM-EDS. These results showed that C, O and Si were predominant elements at all sites. The morphological and chemical analyses indicate that the influence of vehicular emissions as a common source at all sites. The analyses also showed that the urban sites present particles with more diverse morphologies compared to rural and industrial sites.

GAS CHROMATOGRAPHY - MASS SPECTROMETRY ANALYSIS, INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY INVESTIGATION, AND ANTIMICROBIAL SCREENING OF CAESALPINIA BONDUCELLA (L.) ROXB SEED KERNEL

Objective: The objective of this study was to determine heavy metals using inductively coupled plasma mass spectrometry (ICP-MS) and phytochemical constituents of methanol extract of Caesalpinia bonducella seed kernel using gas chromatography - mass spectrometry (GC-MS).&#x0D; Methods: In GC-MS investigation, 95% methanol extract of C. bonducella seed kernel was performed on JEOL GC MATE ΙΙ, column HP 5 MS, and Quadruple, double-focusing mass analyzer. Determination of heavy metals from C. bonducella powder was performed using Thermo scientific I CAP Q instrument, for plant powder digestion Anton Paar Microwave model: Multiwave 300 was used. Antimicrobial activity was evaluated using microdilutions broth method.&#x0D; Results: GC-MS analysis of methanol extract of C. bonducella seed kernel has shown 11 different phytoconstituents. ICP-MS analysis has shown the concentration of ten heavy metals in C. bonducella seed kernel as follows: Cr 1.5 ppm, Fe 72.72 ppm, Co 0.33 ppm, Ni 0.03 ppm, Cu 10.73 ppm, Zn 18.44 ppm, As 0.03 ppm, Cd 0.02 ppm, and Pb 0.58 ppm.&#x0D; Conclusion: Result showed that the plant is safe to use from toxic heavy metals such as As, Cd, and Pb. It is suitable to check frequently the heavy metal content in the plant used in traditional medicines before given to patients.

Zinc and cadmium mapping by NanoSIMS within the root apex after short-term exposure to metal contamination

Zinc as a micronutrient and cadmium as a nonessential toxic element share similar pathways for entering plant tissues and thus may be antagonistic. In nutrient solution culture, 17-day-old radish (Raphanus sativus L) plants were exposed to short-term (24 h) equimolar metal contamination (2.2 µM of each 70Zn and total Cd) to investigate the in situ Zn/Cd distribution in the apical root tissues using high-resolution secondary ion mass spectrometry (NanoSIMS) imaging. Inductively-coupled plasma mass spectrometry analysis of bulk root tissue confirmed large root uptake of both metal elements. After 24-h exposure the total root concentration (in µg/g DW) of 70Zn was 180 ± 24 (mean±SE) and of total Cd 352 ± 11. NanoSIMS mapping was performed on the cross sections of the radish root apex as a crucial component in root growth and uptake of water and nutrients from soil. Elemental maps of 70Zn and 114Cd isotopes revealed greater enrichment of both metals in the outer epidermal root layer than in cortical tissues and especially stele, confirming the epidermal root cells as preferential sites of metal uptake, and indicating relatively slow and less-intensive metal transport into other parts (edible hypocotyl, shoot) of metal-sensitive radish. NanoSIMS has been confirmed as a powerful tool for spatial detection and visualisation of some ultra-trace metal isotopes (e.g. 70Zn) in the fast-growing root tips. However, precise (sub)cellular mapping of diffusible metallic ions (Cd, Zn) remains a technically-challenging task in plant specimens given an unavoidable compromise between optimising methodology for structural preservation vs. authentic in vivo ion localisation.

Studies on hydrometallurgical processes using nuclear techniques to be applied in copper industry. II. Application of radiotracers in copper leaching from flotation tailings

Abstract The use of radiotracers in the present study is intended to replace traditional steps of metal quantitative analysis (solution sampling and instrumental chemical analysis) and to allow real-time measurements of metal concentrations during the leaching process. In this study, 64Cu, an isotope of copper, was selected as a radiotracer. Samples of copper flotation tailings were irradiated in the Maria research reactor (Świerk, Poland) and mixed with an inactive portion of the milled fl otation waste. The leaching process was carried out in a glass reactor, and the radiation spectrum was measured using a gamma spectrometer. The material was then treated using various acids (sulphuric acid, nitric acid, acetic acid, citric acid, and ascorbic acid) in a wide range of their concentrations. Experiments with the radiotracer were conducted in sulphuric and nitric acids. The amount of the leached metal (copper) was calculated on the basis of the peak area ratio in the gamma-ray spectrum of the activated tailings and standard samples. Inductively coupled plasma mass spectrometry (ICP-MS) was also used to analyse the metal content. Maximum recovery of 56% Cu was achieved using 9 M HNO3, whereas the recovery was lowest for ascorbic acid (&lt;1%). Both analytical methods were compared, and the results presented in this paper are in good agreement with radiometric measurements obtained using ICP-MS analysis.

Silica-supported pyrolyzed lignin for solid-phase extraction of rare earth elements from fresh and sea waters followed by ICP-MS detection.

Silica-supported pyrolyzed lignin (pLG@silica) was investigated as a solid sorbent for the pre-concentration of rare earth elements (REE) from natural waters followed by inductively coupled plasma mass spectrometry (ICP-MS) analysis. The carbon-based material was easily prepared by pyrolytic treatment of lignin at 600°C after its adsorption onto silica micro-particles. pLG@silica was characterized by scanning electron microscopy (SEM), surface area measurements (BET method), thermogravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), point of zero charge measurement, and X-ray photoelectron spectroscopy (XPS). The as-prepared material (50mg) was tested as fixed-bed sorbent for the solid-phase extraction (SPE) of tap, river, and sea water samples spiked with REE in the 10-150ngL-1 range, followed by ICP-MS analysis. A quantitative adsorption was observed for all REE with recoveries in the range of 72-118%. A suitable inter-day precision (RSDs 5-12%, n = 3) was obtained. Sample volumes up to 250mL provided enrichment factors up to 100. The method detection and quantification limits (MDLs and MQLs) were in the range of 0.4-0.6ngL-1 and 1-2ngL-1, respectively. The batch-to-batch reproducibility was verified on four pLG@silica independent preparations. As remarkable advantages, pLG@silica proved to be of easy preparation using a waste material, inexpensive, and reusable for at least 20 SPE cycles.

Bromine and iodine determination in human saliva: Challenges in the development of an accurate method

In this work, an analytical method for bromine and iodine determination in human saliva was proposed. A simple protocol based on centrifugation and direct analysis of supernatant by inductively coupled plasma mass spectrometry (ICP-MS) was investigated. Although this method was feasible for bromine determination, iodine was partially present in the supernatant and an agreement about 54% with reference value was obtained. In addition, microwave-induced combustion (MIC) and microwave-assisted dissolution were also evaluated. Using MIC, 0.2 mL of saliva added on 300 mg of microcrystalline cellulose were efficiently digested. A diluted solution (50 mmol L−1 NH4OH) was used for analytes absorption, and a reflux step of 5 min was applied to ensure quantitative recoveries of Br and I. Accuracy was evaluated by analyte recovery experiments, and recoveries between 94% and 98% were obtained. Microwave-assisted dissolution was evaluated for 2.0 mL of saliva using also a diluted alkaline solution (25 mmol L−1 NH4OH) and a microwave irradiation program of 35 min (including the cooling step). Results for this method agreed with those obtained using MIC. Although MIC has also been appropriated for further determination of Br and I in saliva, microwave-assisted dissolution can be considered a simpler sample preparation method and it was effective for high amount of sample (up to 2.0 mL). Moreover, final solutions were compatible with ICP-MS analysis, allowing the quantification of Br and I in human saliva at ultra-trace concentrations (limits of quantification were 0.052 μg mL−1 for Br and 0.022 μg mL−1 for I).

The Effect of Skelp Thickness on Precipitate Size and Morphology for X70 Microalloyed Steel Using Rietveld Refinement (Quantitative X-ray Diffraction)

Precipitates in thin-walled (11 mm) and thick-walled X70 (17 mm) microalloyed X70 pipe steel are characterized using Rietveld refinement (a.k.a. quantitative X-ray diffraction (QXRD)), inductively coupled plasma mass spectrometry (ICP), and energy-dispersive X-ray spectroscopy (EDX) analyses. Rietveld refinement is done to quantify the relative abundance, compositions, and size distribution of the precipitates. EDX and ICP analyses are undertaken to confirm Rietveld refinement analysis. The volume fraction of large precipitates (1 to 4 μm—mainly TiN rich precipitates) is determined to be twice as high in the thick-walled X70 steel (0.07%). Nano-sized precipitates (&lt;20 nm) in the thin-walled steel exhibit a higher volume fraction (0.113%) than in the thick-walled steel (0.064%). The compositions of the nano-sized precipitates are similar for both steels.