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Considering the irreplaceable importance of photocatalytic functionalization reactions and the widespread attention paid to the use of metal–organic frameworks, especially their modified variants, for this purpose in recent years, different types of HKUST-1/POMoW composites were prepared through the immobilization of a series of Keggin-type polyoxometalates (POMs; POW = H3PW12O40, POMo = H3PMo12O40, and POMoW = H3PMo6W6O40) on HKUST-1 as a metal–organic framework (HKUST-1; Cu3(1,3,5-benzenetricarboxilicacid)2). Then, to produce HKUST-1/Cs-POM, the substitution of H+ cations with Cs+ ones as counter cations was carried out. The prepared composites were fully characterized with the PXRD (powder X-ray diffraction), FT-IR (Fourier transform infrared spectroscopy), BET and BJH (sorption of N2), TGA (thermo-gravimetric analysis), SEM (scanning electron microscopy), EDX (energy dispersive X-ray), TEM (transmission electron microscopy), UV-vis DRS (diffuse reflectance UV-vis spectroscopy), photoluminescence (PL) spectroscopy and ICP-AES (inductively coupled plasma atomic emission spectroscopy) techniques. The great importance of the amide functional group and the attractiveness of photocatalytic oxidative functionalization reactions led us to study the formation of this functional group using the prepared catalytic system in line with our previous research in this field. The HKUST-1/Cs-POMoW composite showed a raised photocatalytic performance compared to the discrete components, HKUST-1 and Cs-POMs, in aerobic oxidative amidation of alcohols under illumination with visible light, owing to the presence of catalytically active Cs-POMs deposited on the MOF particles. Besides, the combination of composite components mitigated the recombination rate of the electron–hole pairs, raising its photocatalytic activity. The attractiveness of fluorine solvents for oxidation reactions has led to the study of their role in the efficiency of oxidative amidation of alcohols and their significant effect on the efficiency of the process has been confirmed. The Cu-MOF/POM catalyst showed excellent stability during the reaction, and no significant decrease in its ability was observed during five consecutive cycles.

Pd supported on 5-carboxyoxindole functionalized cell@Fe3O4 nanoparticles (Pd@CAI@cell@Fe3O4), a new magnetic nanocatalyst, was prepared and characterized using inductively coupled plasma atomic emission spectroscopy, Fourier-transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, thermogravimetric analysis, and energy-dispersive X-ray spectroscopy techniques. The synthesized nanocatalyst (Pd@CAI@cell@Fe3O4) was employed for Heck-type arylation of different substituted maleimides with iodoarenes in good to excellent yields. This green catalyst was easily recovered and reused several times with no substantial loss of activity, providing a clean and efficient synthetic procedure with excellent yield and reduced time.

The combination of two-jet arc plasma optical emission spectrometry (TJP-OES) and electrothermal vaporization (ETV) for sample introduction is proposed for the first time. The direct analysis of solid tellurium samples by ETV-TJP-OES is described. The temperature program of ETV enabled the evaporation of the sample matrix (tellurium) and analytes separately. The separate vaporization of the sample matrix and analytes reduced interference, which ensured lower limits of detection of the technique (LODs). The proposed ETV-TJP-OES technique allowed the simultaneous determination of up to 17 elements in a high-purity tellurium sample with LODs ranging from 0.02 to 50 ng g−1. The LODs of Al, Au, Ba, Be, Cr, Mg, Mn, Ni, Pb, Re, Sr and Zn provided by ETV-TJP-OES are 2 to 50 times lower compared with inductively coupled plasma optical emission spectrometry (ICP OES) after sample decomposition and analysis using pneumatic nebulization for sample introduction into the ICP. The accuracy of the proposed technique was confirmed by the analysis of tellurium samples by ICP-OES and by analyte (spike) recovery tests.

Spectroscopic analysis has been considered as a promising tool for the quantitative detection of elements in a biological sample. Inductively coupled plasma optical emission spectrometry (ICP-OES) is an advanced trace element analysis technique that uses the emission spectrum of an excited atom to detect and quantify the element present in the sample.

This study presents the determination of toxic and nutrient elements in vinegar samples using inductively coupled plasma – atomic emission spectrometry (ICP-AES). The determined elements were Pb, N...

Influence of sample pretreatment on the analysis of the high contents of rare earth (REE) and high field strength (HFSE) elements in geological samples by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS) was studied. The rocks and rich ores of the Tomtor Nb-REE deposit were explored. Complete dissolution of the geological samples with a high content of “refractory” minerals has been achieved using fusion with a sodium peroxide. The results obtained by ICP-AES and ICP-MS after chemical dissolution are comparable with the results obtained by the XRF-SR without chemical pretreatment

It has been shown that Grand spectrometers based on a hybrid assembly of BLPP-2000 photodetector arrays produced by VMK-Optoelektronika can be used for atomic emission spectral analysis of solutions using inductively coupled plasma atomic emission spectroscopy (ICP-AES). For the prototype of a Grand-ICP spectrometer consisting of a Grand spectrometer, RF plasma generator, and RF (radio frequency) power supply the following analytical characteristics were determined: element detection limit, long-term stability linear ranges of calibration graphs for several elements, and optimal operating parameters of the RF generator. The linear concentration range of analyte elements is 105 when using a single analytical line of the element. The long-term stability is less than 2% in 6 h without using an internal standard. The detection limits are comparable to those of modern ICP spectrometers with an axial plasma view and lie in a range of sub-microgram per liter. It has been found that the effect of superposition of the spectral lines of the plasma background, for example, OH molecular lines or others, on the analyte lines can be eliminated by subtracting the blank sample spectrum from the analyte spectrum using Atom software. The analytical characteristics of the spectrometer allow the use of the device both for developing new ICP-based systems and for restoring the performance of defective ICP spectrometers.

Very little is known about how the elemental composition (ionome) of an insect cuticle varies as a result of different colouration. Using inductively-coupled plasma optical emission spectrometry (ICP-OES), we established ionomic profiles in microsamples of two adjacent regions of an insect cuticle with a contrasting colour pattern, namely, the black and orange regions of the elytra of the aposematic burying beetle Nicrophorus vespillo. The analysis revealed 53 elements (ranging in atomic weight from Na to Bi) occurring above the detection limit. The frequency of detectability of individual elements varied strongly, and only ten elements (Ba, Cu, Fe, K, Mg, Mn, P, Rb, Sb and Zn) were present in concentrations exceeding the detection limit in all the samples. The sum of concentrations of all elements in the orange regions of the elytra was 9% lower than in the black ones. The opposite distribution was displayed by the rare earth elements (REEs), the sum of which was 17% lower in the black elytral regions than in the orange ones. The concentrations of six elements were significantly higher in the black than in the orange regions: Al (by 97%), Cu (41%), Mn (14%), Na (46%), Se (97%) and W (47%). The concentrations of essential elements measured in both the black and orange regions exhibited very considerable variance: Ca (σ2 = 1834; 1882, respectively), K (145; 82) P (97; 76), Na (84; 53), Mg (24; 26) and Ba (9; 13). This, in part, could be attributed to individual differences, e.g. those resulting from the consumption of animal carcasses of different quality/chemical composition, but interference between elements and the consequent lowering of measurement quality are also possible. We highlight the fact that deeper insight into the basic relationship between insect colouration and variation in elemental composition requires micro-sampling of the homogeneous layers of an exoskeleton.

A robust and reliable analytical procedure for the determination of trace (mg∙kg−1) and ultra-trace elements (μg∙kg−1) in soil and sediments by inductively coupled plasma quadrupole mass spectrometry (ICP-QMS) was optimized. Aliquots of ∼200 mg of two certified reference materials (IAEA Soil-7, soil and IAEA SL-1, lake sediments) were digested in nitric acid (HNO3) purified twice by sub-boiling distillation using a microwave-heated high-pressure autoclave. Incremental addition of tetrafluoroboric acid (HBF4, 0.1–2 mL) to HNO3 was evaluated for yield. The selection of appropriate proportions of digestion acids was crucial to obtain accurate results. Digested samples were analyzed for a range of trace elements including those that are potentially toxic (Ag, Cd, Pb, Sb, and Tl), plant micronutrients (Cu, Fe, Mn, and Zn), those enriched in bitumen (Mo, Ni, and V), and lithophile elements (Al, Ba, Co, Cr, Rb, Sr, Th, Ti, Y, and Zr). Nitric acid alone proved to be sufficient to completely liberate Cd, Co, Cr, Fe, Mn, Ni, Pb, V, and Zn in both soil and sediments (87%–120% recovery). For almost all the other elements, addition of HBF4 was needed for improved recovery. A combination of 3 mL of HNO3 and 1.5 mL of HBF4 was optimal to fully liberate an extended list of elements including Ba, Sb, and Sr from both the reference materials. Conservative lithophile elements (Th, Ti, Y, and Zr) could not be completely recovered with the proposed method, requiring hydrofluoric acid for complete dissolution of recalcitrant minerals.

A technique for analysis of secondary tungsten-containing raw materials (tungsten-containing sludge) using inductively coupled plasma atomic emission spectrometry in combination with microwave autoclave sample preparation has been developed. The composition of the acid mixture and algorithm of microwave heating of the autoclave are chosen to provide a complete quantitative transfer of the sample into a convenient analytical form for subsequent ICP-AES determination of the main components (sample heating to 220°C in the acid mixture of NH 4 F, HNO 3 , and HCl provides a quantitative transfer of the sample components to be determined, into the solution). Analytical lines free from spectral interference were selected to determine Ti, Cr, Fe, Co, Ni, and W We used real industrial samples of secondary raw materials obtained in product manufacture from VK-type hard alloys [solid solution of tungsten carbide grains (WC-phase) in cobalt (Co-phase)], presented in the form of tungsten-containing powders, grinding sludge of solid sintered alloys, dust waste, defective mixtures, waste ventilation systems, and carbide powders. Correctness of the element determination was proved in analysis of ferrotungsten standard samples upon determination of the matrix component (tungsten) and by the methods of additives and sample weight variation upon determination of the alloying elements and impurities. The method of internal standard (with Sc as the element of comparison) was used to improve the precision and accuracy of the tungsten determination. The relative standard deviation was thus reduced from 0.03 to 0.004. The developed precise rapid technique was tested in analysis of industrial samples of secondary tungsten-containing sludge of hard alloys. The technique is recommended to control the composition of the secondary tungsten-containing sludge of hard alloys in a wide range of concentrations.

A planar probe and optical emission spectroscopy were employed to analyze parameters in an inductively coupled plasma (ICP). The analyses were performed in Ar, Ar+SF6 and O2 plasmas at 40 mTorr. Typical probe results indicate an ion current of 10-3 A/cm2 and an electron temperature (high energy tail) between 1-2 eV in measurements at high powers. At low powers a distinct discharge regime is observed, typically with low density (low ion current) and high electron temperature. The optical emission studies also showed the presence of these two regimes. Moreover, the electron temperature determination using this diagnostic is also in good agreement with planar probe results.

Objective : In this study, we have evaluated trace element concentration of various parts of Eicchornia crassipes, collected from three different lakes in Pune district, India.Methods : The dried segregated parts of Eicchornia crassipes were subjected to microwave digestion, followed by measurement with Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) and Inductively Coupled Plasma-Mass Spectroscopy (ICP-MS). Optimization and validation of the method was performed for determining the minor and trace element concentrations of Co, I, Ni, Cu, Mn, Zn, Fe in roots, petiole and leaves of the plant. NIST Standard reference material SRM 1547 (Peach leaves) was used for establishing accuracy of the analytical method. Rhodium was used an internal standard for correcting matrix effects.Results and Discussion : A validated ICP-OES and ICP-MS method was established for determining the minor and trace element concentrations of Co, I, Ni, Cu, Mn, Zn, Fe in roots, petiole and leaves of the plant. Levels of all elements were found to be higher in roots, followed by petiole and leaves. Except for Zn and Fe, where concentration in leaves was found to be higher than in petiole. Of all the measured elements, total concentration of Mn was found to be highest (566 mg kg-1), followed by Fe (341 mg kg-1), Zn (40.26 mg kg-1), Cu (28.04 mg kg-1), Ni (9.54 mg kg-1), Co (4.33 mg kg-1) and I (0.94 mg kg-1). A surprising finding was the presence of iodine in the plant, despite its non-marine source.Conclusion : Plant-derived products form an important category in alternative medicine that is often used for treatment of several disorders. Eicchornia crassipes (water hyacinth), considered as the world’s worst weed, has been used in folk medicine, with very little evidence-based data to support its potential medicinal value. Here we report the trace element profile of Eicchornia crassipes. Insight into the trace element profile of various parts of the plant can perhaps be harnessed to postulate the rationale behind the use of specific parts of the weed in traditional medicine.

A novel ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) based on melting of the donor phase for the determination of Cd, Cu, and Fe in margarine samples using high-resolution continuum source electrothermal atomic absorption spectrometry (HR-CS ET AAS) is proposed. Considering that margarine is in the solid phase at room temperature, requiring heat for melting, the microextraction process was assisted by an ultrasonic bath to ensure the melting point of the samples and to increase the extraction efficiency of the analytes by UA-DLLME. After the extraction procedure, the aqueous phase was collected and directly introduced into a graphite furnace. The procedure was applied for extraction and multi-element determination, exploring the strategy of simultaneous and sequential determination of analytes by HR-CS ET AAS. A low volume of nitric acid solution in the presence of ethanol and hydrogen peroxide allowed the metals to be separated from the sample in an aqueous phase with subsequent determination by HR-CS ETAAS. In the extraction procedure, 5.0 g of each margarine sample was sonicated under heating in the presence of 100 μL of a solution containing HNO3 0.1 mol L−1, ethanol (95.1%, v v−1), and H2O2 3% (v v−1) in a volume proportion of 2:1:1. The influences of the time of extraction, temperature of extraction, and amplitude of sonication were examined, and the proposed conditions were as follows: extraction time, 10 min; temperature, 60 °C; and amplitude, 100%. Using 5 g of margarine sample, limits of detection of 0.03, 0.52, and 224 ng g−1 were obtained for Cd, Cu, and Fe, respectively. Recovery tests were performed, and the results ranged from 87 to 108% for Cd, 91 to 115% for Cu, and 85 to 112% for Fe. The results obtained by the proposed extraction procedure agreed with those obtained after wet digestion of the sample and determination by inductively coupled plasma optical emission spectrometry (ICP OES).

Made available in DSpace on 2021-06-25T10:14:22Z (GMT). No. of bitstreams: 0 Previous issue date: 2021-03-01 Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP) Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq) Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES) In the present study, a minimal-invasive analytical method for determination of Cu, K, Sr, and Zn in cocoa beans was performed using energy X-ray fluorescence (EDXRF) and laser-induced breakdown spectroscopy (LIBS) combined with multivariate calibration. Partial least squares (PLS) chemometric technique was applied to modeling the data, and inductively coupled plasma optical emission spectrometry (ICP OES) technique was the reference method for the chemical elements concentration levels, after microwave acid mineralization. The figures of merit estimated for Cu, Sr, Zn, and K showed good performance, with acceptable trueness values (85–120%). Data fusion strategy between EDXRF and LIBS data was used to enhance the predictive capability of K. In addition, lower standard error of cross-validation (SECV) (872 mg kg−1) was obtained, showing better performance than those obtained by individual data. Group of Applied Instrumental Analysis Department of Chemistry Federal University of São Carlos Group of Alternative Analytical Approaches (GAAA) Bioenergy Research Institute (IPBEN) Institute of Chemistry São Paulo State University (UNESP) National Institute of Alternative Technologies for Detection Toxicological Assessment and Removal of Micropollutants and Radioactive Substances (INCT-DATREM) Group of Alternative Analytical Approaches (GAAA) Bioenergy Research Institute (IPBEN) Institute of Chemistry São Paulo State University (UNESP) FAPESP: 2014/50945-4 FAPESP: 2018/18212-8 FAPESP: 2019/01102-8 FAPESP: 2019/24223-5 CNPq: 305637/2015-0 CNPq: 307328/2019-8 CNPq: 465571/2014-0 CAPES: 88887136426/2017/00 CAPES: Finance Code 001

Fruits contain nutrients, minerals, trace elements, vitamins, and phytochemicals that are important in terms of human health. When fruits are consumed in a balanced diet, they have a positive effect with regard to reducing disease risk. As a result of heavy metal contamination of the environment, they can be a potential source of toxic elements so it is important to determine the toxic, essential, and trace elements in fresh fruit and commercial fruit products such as fruit juice, marmalade. This study aims to determine the concentrations of Al, B, Ca, Cu, Fe, K, Mg, Mn, Na, Zn, P, and S in tropical fruits (tamarind (Tamarindus indica), star fruit (Averrhoa carambola), golden berry (Physalis peruviana), kumquat (Citrus japonica), dragon fruit (Hylocereus undatus), passion fruit (Passiflora edulis)) by using inductively coupled plasma optical emission spectrometry (ICP-OES) after different microwave acid digestion procedures. The efficiencies of digestion in tropical fruit samples were investigated and compared. Six milliliters of HNO3 + 2 mL of H2O2, 6 mL of HNO3 + 2 mL of HCl, 8 mL of HNO3, 8 mL of HNO3 + 4 mL of H2O2 (30%), 8 mL of HNO3 + 4 mL of HCl, and 12 mL of HNO3 were used for microwave acid digestion procedures. Microwave digestion procedures were applied for the analysis of seventy-two tropical fruit samples purchased in triplicate for each tropical fruit and major, toxic, and minor element contents of tropical fruits were determined. The parameters of the merit evaluated were validated according to limits of detection (LOD) and limits of quantification (LOQ), linearity, recovery, and precision. The highest results of LOD and LOQ were found for Ca, K, Na, Mg, and S. The recovery percentages are in the range from 71.01 to 117.31% in tropical fruits. The digestion efficiency was correlated with the residual carbon content, which was determined by total organic carbon analyzer (TOC). Six milliliters of HNO3 + 2 mL of HCl digestion method was chosen as the effective digestion method because of the lowest residual carbon contents and the accuracy results.

Presented here is a novel automated method for determining the trace element composition of bulk thorium by inductively coupled plasma–optical emission spectroscopy (ICP-OES). ICP-OES is a universal approach for measuring the trace elemental impurities present in actinide-rich materials; however, due to the emission rich spectrum of the actinide, a separation from the trace elements is warranted for spectrochemical analysis. Here, AG MP-1 ion exchange resin was utilized for retention of the Th matrix, while allowing the trace element impurities to be separated prior to subsequent analysis using ICP-OES. After demonstrating the separation on traditional gravity-driven columns, the methodology was transitioned to an automated platform for comparison. This automated platform utilizes syringe-driven sample and solvent flow and can collect the trace element and thorium fractions in separate locations. While reducing the sample size (500 µL, 1.5 mg of Th), maintaining the overall separation efficiency (recoveries >95%), and illustrating the sample throughput ability (n = 10+), this automated methodology could be readily adopted to nuclear facilities in which the determination of trace elemental impurities in Th samples is warranted.

This work present the synthesis of Cu (I) immobilized on modified boehmite nanoparticles as an environmentally friendly heterogeneous catalyst for the synthesis of sulfides and their oxidation to the corresponding sulfoxides in good to excellent yields. The structure of the catalyst was studied by scanning electron microscopy, X-ray diffraction, thermogravimetric, inductively coupled plasma atomic emission spectroscopy, and Brunauer–Emmett–Teller techniques. The use of this heterogeneous nanocatalyst in mentioned organic reactions allowed achieving good results such as the excellent stability, high efficiency, low cost, easy recovery, and reusability of catalyst for four continuous cycles.

Pd(0) nanoparticles stabilized over polydopamine (PDA) capped magnetic GO/Fe3O4 nanocomposites (GO/Fe3O4@PDA/Pd) have been synthesized in variable Pd load following a post grafting approach. Pd has been reduced in situ by the functionalized PDA avoiding the use of external harsh reductant. The structural properties of the synthesized materials were studied by different analytical techniques like Field Emission Scanning electron microscopy (FESEM), Energy Dispersive X-ray Spectroscopy (EDX), High Resolution Transmission Electron Microscopy (HRTEM), Fourier Transformed Infrared (FT-IR) spectroscopy, Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES), Thermo Gravimetric Analysis (TGA), Powder X-Ray Diffraction (XRD) and X-ray Photoelectron Spectroscopy (XPS). The novel GO/Fe3O4@PDA/Pd(0) nanocomposite exhibited excellent performance as a reusable catalyst in the facile cyanation of aryl halides using K4[Fe(CN)6] as a low cost and safe cyanating agent. The aryl nitriles were obtained in good to excellent yields and the catalyst was recycled up to 13 times with minimal change in its catalytic activity.

Manganese (Mn) contained in cellulose is partially responsible for an increased consumption of paper bleaching chemicals (like O2, H2O2), consequently diminishing the efficiency in pulp processing, darkening the pulp and deteriorating pulp quality. Usually, Mn in the paper industry is removed employing the environmentally critical EDTA. A greener alternative constitutes, however, the use of siderophores, high-affinity metal-chelating organic compounds that are produced by microorganisms to acquire metals (Fe and Mn among others), like desferrioxamine B (DFOB) or desferrioxamine E (DFOE). The use of native Mn-transporter proteins, like PratA, constitutes another possibility for Mn removal. The evaluation of utilizing siderophores or PratA for Mn removal from cellulose in a circular economy scheme is therefore essential. Firstly, Mn removal from cellulose was performed by immobilizing siderophores or PratA on magnetic beads (M-PVA C22). Secondly, the beads were incubated overnight with a 2% cellulose suspension, allowing Mn-ligand complex formation. Finally, cellulose suspensions were submitted for Mn quantification, employing either the TCPP [Tetrakis(4-carboxyphenyl)porphyrin] method, the PAN [1-(2-pyridylazo)-2-naphthol] method or the Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). When non-immobilized ligands were employed, a 31% Mn removal was achieved; when using immobilized ligands, around 10% Mn removal was obtained. Treated and untreated cellulose was analyzed by SEM and the Mn distribution between the solid and liquid phase was parameterized using adsorption isotherm models. This novel greener method proved to be feasible and easy, leading to potential improvements in the paper industry. Next research steps are to optimize Mn removal and quantify Mn recovery after ligand decoupling before scaling-up.

The most trace metals (essential and toxic metals) in very low concentrations are needed for living organisms, especially humans, but if they exceed the recommended limit, they can lead to toxicity...

In this study, the mineral and heavy metals (arsenic (As), cadmium (Cd), copper (Cu), iron (Fe), mercury (Hg), potassium (K), manganese (Mn), sodium (Na), phosphorus (P), and lead (Pb)) in two red Tunisian seaweeds Gymnogongrus griffithsiae (G. griffithsiae) and Asparagopsis taxiformis (A. taxiformis), were evaluated. Mineral and trace element analyses were achieved using inductively coupled plasma optical emission spectrometry (ICP-OES). Fourier transform infrared (FTIR) spectroscopy was used to predict the major functional groups that would be implicated in the seaweeds mineral uptake. Our results showed that the studied A. taxiformis species had much higher mineral and heavy metal concentrations than G. griffithsiae. Na (200.60 mg/kg) was the most abundant element followed by K (137.84 mg/kg) > P (35.93 mg/kg) for A. taxiformis species. However, only Na (165.23 mg/kg) and P (51.19 mg/kg) were detected in G. griffithsiae alga. As regards heavy and toxic metals, allowable concentrations have been found in both seaweeds. The concentration ranges for the most undesirable heavy metals were as follows: Pb (0.39-0.51 mg/kg), As (0.11-0.40 mg/kg), Cd (0.01-0.02 mg/kg), and Hg (0.00-0.02 mg/kg). According to FTIR analysis, the major functional groups present in the studied seaweeds were carboxyl, hydroxyl, sulfate, and phosphate groups that are considered as excellent binding sites for metal retention.

In this study, on-line ultrasound-assisted dispersive micro-solid phase extraction technique is introduced for the separation and ICP-OES determination of thorium in aqueous samples. In this method, microparticles of g-C3N4 were dispersed into the sample using ultrasonic radiation and Th(IV) ions were directly adsorbed by the sorbent. The sample solution was then passed through a membrane filter and the adsorbed Th(IV) ions were subsequently eluted directly into the ICP-OES nebulizer. The Limit of detection of developed method was 0.05 μg L−1. The developed on-line technique eliminates the centrifugation step in order to simplify and speed up the extraction procedure.

Worldwide, medicinal plants and herbal medicines are widely consumed. The aim of this study was to determine macro- (Ca, K, Mg, Na, and P) and microelements (Al, As, Ba, Cd, Co, Cr, Cu, Fe, Mn, Mo, Ni, Pb, Sb, Se, Si, Sn, Sr, V, and Zn) in medicinal plants and herbal medicines: “globe artichoke” - Cynara scolymus L., “devil’s claw” - Harpagophytum procumbens D.C., and “espinheira santa” - Maytenus ilifolia (Mart) ex Reiss. Concentrations of 24 (essential and toxic potentially) elements in samples from Brazil were determined using a sequential optical emission spectrometer with inductively coupled plasma optical emission spectrometry (ICP OES) after acid digestion, assisted by microwave radiation. Principal component analysis (PCA) and hierarchical cluster analysis (HCA) were used to carry out an exploratory analysis of samples. The elements were quantified (in μg/g): Al (20.24–1261.64), Ba (18.90–63.18), Ca (2877.6–19,957.40), Cr (0.28–1.38), Cu (4.16–21.99), Fe (8.54–627.49), K (1786.12–32,297.19), Mg (505.82–6174.52), Mn (0.40–205.64), Na (1717.23–18,596.45), Ni (< LoQ–0.99), P (35.12–2899.91), Se (1.52–3.71), Sn (1.53–12.43), Sr (52.33–84.31), V (< LoQ–0.24), and Zn (2.60–30.56). As, Cd, Co, Mo, Pb, and Sb, in all the investigated samples, were found to be below the limit of detection (LoD) and quantification (LoQ) values of ICP OES. These medicinal plants and herbal medicines can be sources of Ca, K, Mg, Na, P, Cu, Fe, Mn, Se, and Zn. All samples showed considerable levels of Al. PCA and HCA showed that the samples separated into two large groups.

This study presents the results of the iron oxide content determination in bauxite by means of inductively coupled plasma optical emission spectrometry (ICP-OES), volumetry, and UV–VIS spectrophotometry. Nine certified bauxite reference samples with Fe2O3 content from 7.14 to 28.20% were analyzed. Two methods of bauxite sample preparation were applied: melting with a mixture of Na2CO3:Na2B4O7 (3:1) and dissolving with a combination of acids (HCl, HNO3, and H2SO4). The recovery value for all the methods used in relation to the certified values was in the range from 92.41% to 113.87%. By using statistical tests, it has been confirmed that the results of ICP-OES analysis generally agree with other methods, which supports its adoption as an alternative for Fe2O3 determination in bauxite. Due to a shorter preparation time and complete dissolution, it is recommended to prepare the samples by melting.

Several pathologies, such as cancer, predispose the depletion of nutritional status, which makes it essential to offer a balanced diet, which highlights the role of minerals, due to their relevance in contributing to the treatment and recovery of patients. The objective of the study was to determine the levels of calcium (Ca), potassium (K), magnesium (Mg), sodium (Na) and phosphorus (P) in hospital meals (general, bland and pasty) and in an additional meal called complement oral food (CAO) that contained foods with added proteins, carbohydrates and / or fibers, and also evaluate the suitability of each macromineral in relation to nutritional recommendations (DRIs). Samples were collected in duplicate from six daily meals and from CAO on two non-consecutive days, from a hospital in Belo Horizonte (MG). Macrominerals were determined by an optical emission spectrometer with inductively coupled plasma (ICP OES). Statistical analyzes were performed using Stata 11.0 and the statistical significance was established as p

Antimony (Sb) is a redox-sensitive toxic trace metalloid that occurs just below arsenic (As) in Group 15 of the periodic table. These two elements share many geochemical and toxicological similarit...

The evaluation of the migration of metallic elements in the metal containers is usually performed through the direct analysis of the cans’ content. However, this may be biased by exogenous factors ...

The presence, concentration and distribution of 42 trace and ultra trace elements in addition to rare earth elements (REE), yttrium(Y) and Thorium (Th) were analyzed using Inductively coupled plasma optical emission spectrometer (ICP-OES) in different body parts and organs of Japanese quail Cotornix japonica as a laboratory animal model. Twenty one of the investigated elements were below detection limit while the rest of the investigated elements varied in amount and distribution relative to organs and parts in which they were investigated. The existences, concentrations and distributions of Thallium (Tl) and europium (Er) are recorded in a higher living species by the present work. The present work also documented presence, concentration and distribution of Thulium (Tm) a living organism. The recorded concentrations and distributions of various elements may be related to their roles in structures and functions of organs in which they were distributed. From the present findings, we recommend better classification of elements according to distribution and concentration levels in individual organs. We also recommend investigation of the existence of Tm, Tl, and Er in other living species. We also recommend further investigation in the role of Tm, Tl, and Er in structure and metabolism of C. japonica parts and organs in which they were detected

Ground water is continuously monitor and observed for drinking purposes so that risk from contaminants can be reduced by appropriate treatment methods. In the study area 25 ground water were collected from upstream to downstream of Sukhna River in Aurangabad city to evaluate the heavy metal concentration during post monsoon season in December 2016 with help of Inductively Coupled Plasma- Optical Emission Spectroscopy (ICP-OES). It is based on emission technique with high accuracy and precision for analyzing heavy metals to trace metals level concentration in water. Total 25 samples were subjected to analysis for eight heavy metals like Lead, Nickel, Zinc, Arsenic, Chromium, Copper, Manganese, iron using this technique. Expect Zinc and Nickel concentrations, levels of remaining heavy metals in all samples are higher than Bureau of Indian standard.

A new online vortex-assisted dispersive micro-solid phase extraction method was developed for the preconcentration of trace amounts of indium as a prior step to its determination by inductively cou...

Toxic heavy metal pollution of water is a major environmental problem and the current remediation approaches are not optimal as they are non-eco-friendly and lacking in efficiency. As such phytoremediation, a green remediation technology is recognized as a better approach. In this study, both Fourier Transform Infrared (FTIR) Spectroscopy and Inductive Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) were used to investigate the capability of an aquatic plant, water hyacinth (

Aqueous zinc-ion batteries and capacitors are potentially competitive grid-scale energy storage devices because of their great features such as safety, environmental friendliness, and low cost. Herein, a completely new phenanthroline covalent organic framework (PA-COF) was synthesized and introduced in zinc-ion supercapatteries (ZISs) for the first time. Our as-synthesized PA-COF shows a high capacity of 247 mAh g–1 at a current density of 0.1 A g–1, with only 0.38% capacity decay per cycle during 10 000 cycles at a current density of 1.0 A g–1. Although covalent organic frameworks (COFs) are attracting great attention in many fields, our PA-COF has been synthesized using a new strategy involving the condensation reaction of hexaketocyclohexanone and 2,3,7,8-phenazinetetramine. Detailed mechanistic investigations, through experimental and theoretical methods, reveal that the phenanthroline functional groups in PA-COF are the active zinc ion storage sites. Furthermore, we provide evidence for the cointercalation of Zn2+ (60%) and H+ (40%) into PA-COF using inductively coupled plasma atomic emission spectroscopy and deuterium solid-state nuclear magnetic resonance (NMR). We believe that this study opens a new avenue for COF material design for zinc-ion storage in aqueous ZISs.

The consumption of ayahuasca, a brew prepared from the decoction of two Amazon plants, has increased worldwide in the last decades. This fact raised questions about the safety in its oral administration. In this sense, information concerning the chemical composition of ayahuasca is essential to find a comprehensive reply. Therefore, the aim of this study consisted of determining the elemental composition of ready-to-consume ayahuasca samples produced in Brazil, in order to evaluate the safety in the oral administration of this beverage, considering recommended macroelement and microelement daily intake values and the permitted limits of potentially toxic heavy metals. Real ayahuasca samples, obtained from Brazilian religious groups, underwent microwave radiation-assisted acid decomposition, and Li, Al, Mn, Fe, Co, Cu, Zn, As, Cd, Hg, and Pb concentrations were determined by ICP-MS, while Ca, Mg, K, and P concentrations were determined by ICP OES. Method accuracy was assessed by analyte addition and recovery assays. Recoveries ranged from 80 and 118%, indicating satisfactory accuracy. Limit of detection (LOD) and limit of quantification (LOQ) values were lower than 1 mg L−1 for the macroelements determined by ICP OES and lower than 3.5 μg L−1 for the microelements determined by ICP-MS. The concentrations of the elements determined in the samples were lower than the recommended or tolerable limits; hence, it is possible to affirm that ayahuasca presents safe administration levels regarding total elemental content.

Introduction: In recent years, the contamination of food with heavy metals has received much attention. Plants can absorb metal pollutants through contaminated water, soil, and air. Materials and Methods: In the current study, accumulation of minerals in three types of soybeans was investigated by wet and dry digestion methods using ICP-OES technique. Thereafter, the metals' health risk was assessed by estimated daily intake, toxic hazard quotient (THQ), and hazard index (HI) values. Results: According to the results, the concentrations of Cr, Se, Ca, Fe, Mo, Mn, and Mg in soybean seeds were 0.034-170.88 mg/kg, 0.21-243.79 mg//kg, 2.50-33.37 mg/kg, 0.05-0.86 mg/kg, 0.071-203.57 mg/kg, 0-0.47 mg/kg, and 2.69-19.31 mg/kg, respectively. The ashing method had a better performance in determining Ca, Fe, Mo, Mn, and Mg concentrations than the wet digestion method. The THQ rates were below 1 for the three varieties of each mineral element, but the HI values of variety 2 and variety 3 were higher than 1 in both methods. Conclusion: Furthermore, continuous monitoring of the soybeans' mineral and heavy metal contents seems necessary

Siddha system of medicine is practiced in regions of South India. The eighteen Siddhars were the men who achieved supreme knowledge in the field of medicine, yoga and tap, since then this system of medicine developed. Acalypha indica is an important medicinal plant mentioned in Siddha literature. In the present study, Charu prepared from raw powder of leaves of this plant were evaluated by using different techniques like Fourier Transform Infrared (FTIR) Spectroscopy analysis for determination of associated functional group, Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) for the quantification of trace and heavy elements and antifungal activity of Charu were tested. FTIR analysis showed the broad peaks for numerous functional groups like alkanes, alkynes, alkyl halide, aromatics, alkaloid etc. Elemental analysis from this plant shows good results for most of trace as well as heavy elements which have great significance in diet. Plant product Charu shows good antifungal activity against four different pathogenic skin disease causing fungi and hence the formulation can be used to treat dermal infections.

The aim of this study is to demonstrate a valid and simple extraction method for the extraction of heavy metals from olive oil and its quantitative determination by ICP-AES technique. Fifteen olive oil samples are collected from different manufacturing companies originates from five countries. Fourteen metals are quantitively detected in all samples including; Aluminum, Arsenic, Calcium, Cadmium, Cobalt, Chromium, Copper, Iron, Potassium, Magnesium, Manganese, Nickel, Lead and Zinc. A simple extraction method has been proposed for the extraction of heavy metals from the raw oil samples based on diluted 10% HNO3. Test method validation procedures have been carried out for the quantitative analytical determination of the detected trace metals in the investigated oil samples. The trace elements are found to be in the concentration range from 0.0001 to 8.39 mg.kg-1. As a result of the test method validation; linearity (R2) is above 0.99, the recovery ranged between (72.63% to 124.62%), the limit of detection and the limit of quantitation are between (0.006– 2.32 µg.kg-1) and (0.022 – 7.68 µg.kg-1) respectively. The relative standard deviation (RSDs) for repeatability and ruggedness are found to be lower than 2.2% for selected elements, which confirms the precision of the ICP-AES analytical method. The results demonstrate the validity of accurate, precise, rugged, selective, specific and stable ICP-AES determination method for trace metal analysis in raw olive oil samples that based on the proposed simple extraction method.

Measurement uncertainty (MU) associated with the determination of the light rare earth elements (La, Ce, Pr, Nd, Sm, Eu), yttrium and uranium in different types of rock samples by an ICP-OES method has been evaluated by the three principal approaches: the GUM modelling approach, the Nordtest single laboratory approach and the Horwitz equation. A within-laboratory validation data for specificity, linearity, range, accuracy and precision was used for the MU calculations. Procedures have been described for the MU calculations by the three approaches and MU results for an in-house rock sample by the three approaches have been compared. MU results by the GUM approach were in good agreement with those obtained using the Horwitz equation, but were lower than those obtained by the Nordtest approach.

Calibration by the concentration ratio provides better metrological characteristics compared to other calibration modes when using the inductively coupled plasma atomic emission spectrometry (ICP-AES) for analysis of geological samples and technical materials on their base. The main reasons for the observed improvement are: i) elimination of the calibration error of measuring vessels and the error of weighing samples of the analyzed materials from the total error of the analysis; ii) high intensity of the lines of base element; and iii) higher accuracy of measuring the ratio of intensities compared to that of measuring the absolute intensities. Calcium oxide is better suited as a base when using calibration by the concentration ratio in analysis of carbonate rocks, technical materials, slags containing less than 20% SiO2 and more than 20% CaO. An equation is derived to calculate the content of components determined in carbonate materials when using calibration by the concentration ratio. A method of ICP-AES with calibration by the concentration ratio is developed for determination of CaO (in the range of contents 20 – 100%), SiO2 (2.0 – 35%), Al2O3 (0.1 – 30%), MgO (0.1 – 20%), Fe2O3 (0.5 – 40%), Na2O (0.1 – 15%), K2O (0.1 – 5%), P2O5 (0.001 – 2%), MnO (0.01 – 2%), TiO2 (0.01 – 2.0%) in various carbonate materials. Acid decomposition of the samples in closed vessels heated in a HotBlock 200 system is proposed. Correctness of the procedure is confirmed in analysis of standard samples of rocks. The developed procedure was used during the interlaboratory analysis of the standard sample of slag SH17 produced by ZAO ISO (Yekaterinburg, Russia).

A modified calibration curve method based on the combination of standard addition and traditional calibration curve methods was employed for the quantification of Prussian blue nanoparticles in rat...

Rare earth element (REE) contamination has major consequences for the environment and humans. Some forms of REEs have more serious environmental impacts than others. It is thus crucial to monitor their levels in areas where they are expected to be released. Concentrations of 13 REEs (La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu) around the Barakah nuclear power plant (NPP) area, Abu Dhabi, United Arab Emirates (UAE), were measured. Shore, soil, and marine samples were collected. REE concentrations were measured using inductively coupled plasma atomic emission spectroscopy. On average, REE concentrations were highest in the soil samples, followed by the marine samples and then the shore samples. La and Nd were the most abundant REEs in the soil, marine, and shore. The average (La/Yb)n ratios for shore, soil, and marine samples were 8.96, 9.75, and 9.39, respectively. The REE concentrations were strongly positively correlated with Al2O3 values, suggesting low mobility of the REEs in the Barakah NPP area. Light REEs (LREEs) were more enriched than heavy REEs (HREEs). The shore samples have minor enrichments in La and Tm. Otherwise, based on enrichment factors that do not exceed 1.2 and geoaccumulation indices that were all below zero, the Barakah NPP area was considered uncontaminated with REEs. This area was not polluted according to the pollution load indices (0.67, 0.52, and 0.17 for shore, soil, and marine sediments, respectively). The spatial distribution maps show the highest concentrations of REEs in the south area of the Barakah NPP. Overall, the Barakah NPP area does not have any alarming REE concentrations, and the baseline values were provided as a reference for future comparisons.

The main aim of the present study was to investigate the effects of ultrasonic irradiation on thermophysiological comfort properties of TiO2-coated fabrics. The results were evaluated on the basis of heat and mass transfer as well as air permeability performances. Alambeta, a permetester, an air permeability tester, and a moisture management tester were used for thermal evaluation and air and moisture transportation, respectively. Hundred percent pure cotton and polyester woven fabrics were used for this study. Moreover, the study explains the effect of sonication on surface roughness of textile woven fabrics. TiO2 nanoparticles were deposited onto selected fabrics by sonication. Surface topography, changes regarding surface roughness, and the presence of nano TiO2 were evaluated by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) analysis, X-ray diffractometry (XRD), and inductively coupled plasma atomic emission spectroscopy (ICP-AES). Furthermore, standard test methods were carried out to evaluate physical and overall thermophysiological comfort properties, i.e., thermal conductivity, thermal absorptivity, relative water vapor permeability, absolute evaporative resistance, air permeability, and overall moisture management capacity of TiO2-treated and untreated samples.

In the present work a method was proposed for the direct determination of Ca, Fe, K, and Mg and qualitative analysis of anthropized and cabruca soil samples from different depths (0–20 and 20–40 cm) by laser-induced breakdown spectroscopy (LIBS). The LIBS instrumental parameters were evaluated using a central composite design with a central point. The variables evaluated were as follows: delay time in five levels (0.5, 0.7, 1.2, 1.7, and 1.9 μs) and fluence at five levels (1448, 1811, 2659, 3514, and 3820 J·cm–2). The best results obtained were with a delay time of 1.2 μs and fluence of 2659 J × cm–2. The proposed calibration model for Ca, Fe, K, and Mg obtained using LIBS data presented a good correlation with the reference values obtained by inductively coupled plasma atomic emission spectrometry (ICP OES). In addition, multivariate data analysis from LIBS spectra in the region of 186–1042 nm was performed using principal component analysis (PCA). From the LIBS spectra it was possible to discriminate the different analyzed samples, showing that the combination of LIBS with PCA is an excellent option for the discrimination of soils.

As consumer awareness of heavy metal content in textile increased, it is necessary to develop analytical methods that identify and quantify heavy metals. In order to comprehensively investigate the potential risks of antimony (Sb) in recycled polyester fiber to humans health, this study developed acid digestion method, with the condition that the volume ratio of concentrated sulfuric acid to hydrogen peroxide was 1, and digested at 200°Cfor 1.5h, which produced clear and colorless solutions.Currently, microwave and dry ashing are also common methods for digesting polyethylene terephthalate samples. Three pretreatment methods for determining the content of Sb in recycled polyester fibers was evaluated. Results showed that inductively coupled plasma-optical emission spectrometry (ICP-OES) analysis of acid digested recycled polyester samples resulted in Sb content higher than for the microwave and dry ashing digestion methods which incompletely digest recycled polyester. Moreover, compared with microwave digestion and dry ashing, acid digestion had a low detection limit of 0.0116 ug/mL, a high spike recovery of 82% to 106% and the RSD value less than 2%, which indicates that the data was accurate and reproducible. Therefore, in this study, acid digestion - ICP-OES was an effective method for detecting the content of heavy metal Sb in recycled polyester.

The refractory lining in a furnace is always damaged and peels off when spent lithium-ion secondary batteries (LIB) are pyro-processed in a rotary kiln. To develop highly durable refractories and to elucidate the erosion behavior, various analyses such as scanning electron microscopy/energy dispersive X-ray spectroscopy, laser-induced breakdown spectroscopy, inductively coupled plasma atomic emission spectroscopy, ion chromatography, and X-ray diffraction were performed on the linings sampled from different sections of a refractory. Our results suggested the following mechanisms in Al2O3–SiO2–CaO refractory damage during pyro-processing of spent LIB packs. First, Li2O, P2O5, LiF, and HF were formed by thermal decomposition of electrolyte constituents of the lithium-ion secondary batteries. When HF reacts with SiO2, Al2O3, and CaO on the surface of the refractory, each fluoride that forms vaporizes and melts. When Li2O and P2O5 (as well as LiF) react with the Al2O3–SiO2 refractory, an Li2O–Al2O3–SiO2–P2O5(-LiF) phase with a low melting point forms and penetrates into the refractory through pores, grain boundaries, and cracks, resulting in peeling off.

Information on the mineral composition of geopropolis produced by bees native to the Amazon region is of great importance for the chemical characterization of this product. This study aimed to dete...

Inductively coupled plasma is a new technique employed for the determination of elemental impurities in pharmaceutical ingredients viz. raw materials, drug substance, and drug product dosage forms. New US FDA and EMA regulations came into effect from Jan 2018 as industry standard requirements for the determination of inorganic elemental impurities using ICP-OES/AES or ICP-MS analytical techniques. The method development was optimized for the determination of the listed elements as per USP elemental impurities-limits and procedures. It also demonstrates the validation of the method and verification/transfer of the method which also provides an insight into the presence of free elemental atomics of the gaseous form of the sample (drug substance, drug product or excipients), thus helping in determining the concentration of the element of interest. Also, the regulatory guidance is very general and does not explain the sample specifications for the individual element concentrations. Thus, this review emphasizes the routine instrumental maintenance, analytical method development challenges, trends in the performance of analytical method validation and verification/ transfer activities of the various pharmaceutical dosage forms outlined with acceptance criterion.