Coupled Plasma Atomic Emission Spectrometry Research Articles

Evaluation of an Inductively Coupled Plasma–Atomic Emission Spectrometry (ICP-AES) Method for the Determination of Macro and Microelements in Trifolium L. Species

This study aimed optimizes the inductively coupled plasma–atomic emission spectrometry (ICP-AES) conditions for the determination of macro and microelements in the flowers and leaves of Trifolium species. After the optimization of instrumental parameters, plasma robustness was achieved under the following conditions: RF power 1350 W, nebulizer flow rate 0.5 L min−1, coolant gas flow rate 12 L min−1, auxiliary gas flow rate 0.5 L min−1, flush pump rate 100 rpm, analysis pump rate 50 rpm, sample flow 0.5 mL min−1, and sample uptake delay 30 s. The limits of detection (LOD) and limits of quantification (LOQs) were lower than literature values. The most abundant microelement in leaves is Ca, followed by K, Mg, P, and Na, and in flowers was K, followed by Ca, P, Mg, and Na. The average contents of microelements decreased in the orders S > Fe > Si > Al > Zn > Mn > Cu > Ni > Co > Pb > Cr > As > Cd for flowers and S > Fe > Si > Mn > Al > Zn > Cu > Ni > Co > Pb > Cr > As > Cd for leaves. Chemometrics were used for grouping samples based upon the elemental contents.

Solidification Kinetics of an Al-Ce Alloy with Additions of Ni and Mn

Heat-treated aluminum–silicon (Al-Si)-based alloys have dominated the cast lightweight alloy industry for several decades. However, in the last decade, Al-Ce-based alloys have shown promise in replacing Al-Si alloys as they remove the need for costly heat treatments. As the properties of Al-Ce alloys depend on the as-cast microstructure, it is important to characterize the solidification kinetics of these alloys. Therefore, this study focused on characterizing the solidification of an Al-Ce alloy with additions of Ni and Mn (nominal composition Al-12.37Ce-3.26Ni-0.94Mn-0.12Fe in weight percent). The alloy was cast in a wedge mold configuration, resulting in cooling rates between 0.18 and 14.27 °C/s. Scanning electron microscopy (SEM) coupled with the energy dispersive x-ray spectroscopy (EDS) and differential scanning calorimetry (DSC) techniques characterized the evolution rate of solid phases. The SEM/EDS data revealed that an Al10CeMn2 phase was present at higher cooling rates. At lower cooling rates, near the center of the casting, a primary Al23Ce4Ni6 phase was more present. It was observed that up to 2.6 atomic percent (at.%) of Mn was dissolved in this primary Al23Ce4Ni6 phase, thereby removing a large portion of the available Mn for forming the Al10CeMn2 phase. DSC analysis showed differences in the samples’ liquidus temperatures, which indicated compositional variations. Inductively coupled plasma–atomic emission spectroscopy (ICP-OES) and Scheil solidification simulations correlated the compositional differences with phase formation, which agreed with the SEM and DSC results. This experiment provides insight into novel Al-Ce-Ni-Mn alloys and where their potential lies in industrial applications.

Thermodynamic and CFD analysis of recycling Cu-As-containing filter cake waste and black copper sludge by feeding them back into FSF

The Cu-As-containing filter cake waste and black copper sludge are the main by-products, besides sulphuric acid and slag, in the copper production. To achieve sustainability in copper making and satisfy more strict environmental requirements, this study discusses the possibility of feeding them back into the smelting step. By collecting samples of filter cake waste and black copper sludge from copper industry, followed by Inductively Coupled Plasma-Atomic Emission Spectroscopy, X-ray Diffractometry and Scanning Electron Microscopy-Energy Dispersive X-ray Spectrometry, the mineralogy, morphologies and compositions of filter cake and black copper sludge were determined. Furthermore, the reaction mechanism of the by-products in FSF was discussed from thermodynamic aspects. Finally, a CFD simulation was conducted on an industrial furnace scale using different copper concentrate/by-product ratios, and the pyrometallurgical recycling of the filter cake waste and black copper sludge were discussed and evaluated.

Addressing the voltage and energy fading of Al-air batteries to enable seasonal/annual energy storage

Al-air batteries are promising candidates for seasonal and annual energy storage. However, severe voltage decay upon discharge limits their practical specific energy. Herein, we first explore the effect of different Al(OH)4− concentrations in alkaline electrolytes on the electrochemical oxidation of Al metal anodes (AMAs). Simulation analysis on the electrochemical impedance spectra of AMAs reveals that the formation of Al(OH)4− reduces the OH− concentration and negatively affects the reaction kinetics of AMAs, which is responsible for increased potentials of AMAs and the consequent voltage decay of Al-air batteries. Subsequently, a seeded precipitation process taking advantage of the lower solubility of Al(OH)4− at 20 °C than at 50 °C is proposed to recover the voltage decay of Al-air batteries. Inductively coupled plasma atomic emission spectroscopy demonstrates that more than 70 wt % of Al(OH)4− in the electrolyte can be removed via this process. Raman spectra and ionic conductivity tests of the electrolyte, together with X-ray diffraction of the precipitate, reveal that the removed Al(OH)4− is converted into insoluble Al(OH)3 with release of OH−. Making use of the precipitation process, Al-air prototypes of Ah-level delivering 3.95 kWh kgAl−1 at 50 mA cm−2 and 3.52 kWh kgAl−1 at 100 mA cm−2 are demonstrated.

Fractal characteristics of artificially matured lacustrine shales from Ordos Basin, West China

Nanometer scaled pores are critical to studying gas shale reservoirs. In order to obtain the information of the evolution mechanism of nanoscale pore within lacustrine organic-rich shales, artificially matured shale samples from the Ordos Basin were treated using hydrous pyrolysis experiment. Low-temperature nitrogen adsorption, inductively coupled plasma atomic emission spectrometry (ICP-AES), and field emission scanning electron microscopy (FE-SEM) experiments were used to investigate the nanopore evolution with migration and precipitation of materials. The results show that the pore sizes were distributed from 1.1 to 500 nm, and the overall porosity tends to increase first and then decrease. The micropores and fine mesopores (< 10 nm) increased gradually from the 250 to the 350 °C, calcite appeared dissolution following a small peak of feldspar dissolution at this stage, and the CO2 reaches a partial pressure peak at 350 °C. The micropores, mesopores and macropores increased steeply from the 370 °C to the 450 °C. Organic pores were not developed until 350 °C, and well developed at 370 and 400 °C. Organic pores, intergranular pores of clay and intragranular pores of pyrite were well developed at 370 °C. The cumulative specific surface areas increased at 400 °C caused by the dehydration and transformation reaction of clay minerals. This study could provide a reference for the exploration of shale gas in lacustrine shales with different thermal maturities.

Origin Traceability of Tobacco Leaves by Multi-elements Analysis Using Inductively Coupled Plasma Atomic Emission Spectroscopy and Cluster Analysis

Origin Traceability of Tobacco Leaves by Multi-elements Analysis Using Inductively Coupled Plasma Atomic Emission Spectroscopy and Cluster Analysis

The Trace Element Concentrations and Oxidative Stress Parameters in Afterbirths from Women with Multiple Pregnancies.

The aim of this study was to evaluate the intensity of oxidative stress by measuring the concentrations of lipid peroxidation products (LPO) in fetal membrane, umbilical cord, and placenta samples obtained from women with multiple pregnancies. Additionally, the effectiveness of protection against oxidative stress was assessed by measuring the activity of antioxidant enzymes, including superoxide dismutase (SOD), catalase (CAT), glutathione peroxidase (GPX), and glutathione reductase (GR). Due to the role of iron (Fe), copper (Cu), and zinc (Zn) as cofactors for antioxidant enzymes, the concentrations of these elements were also analyzed in the studied afterbirths. The obtained data were compared with newborn parameters, selected environmental factors, and the health status of women during pregnancy to determine the relationship between oxidative stress and the health of women and their offspring during pregnancy. The study involved women (n = 22) with multiple pregnancies and their newborns (n = 45). The Fe, Zn, and Cu levels in the placenta, umbilical cord, and fetal membrane were determined using inductively coupled plasma atomic emission spectroscopy (ICP-OES) using an ICAP 7400 Duo system. Commercial assays were used to determine SOD, GPx, GR, CAT, and LPO activity levels. The determinations were made spectrophotometrically. The present study also investigated the relationships between trace element concentrations in fetal membrane, placenta, and umbilical cord samples and various maternal and infant parameters in women. Notably, a strong positive correlation was observed between Cu and Zn concentrations in the fetal membrane (p = 0.66) and between Zn and Fe concentrations in the placenta (p = 0.61). The fetal membrane Zn concentration exhibited a negative correlation with shoulder width (p = -0.35), while the placenta Cu concentration was positively correlated with placenta weight (p = 0.46) and shoulder width (p = 0.36). The umbilical cord Cu level was positively correlated with head circumference (p = 0.36) and birth weight (p = 0.35), while the placenta Fe concentration was positively correlated with placenta weight (p = 0.33). Furthermore, correlations were determined between the parameters of antioxidative stress (GPx, GR, CAT, SOD) and oxidative stress (LPO) and the parameters of infants and maternal characteristics. A negative correlation was observed between Fe and LPO product concentrations in the fetal membrane (p = -0.50) and placenta (p = -0.58), while the Cu concentration positively correlated with SOD activity in the umbilical cord (p = 0.55). Given that multiple pregnancies are associated with various complications, such as preterm birth, gestational hypertension, gestational diabetes, and placental and umbilical cord abnormalities, research in this area is crucial for preventing obstetric failures. Our results could serve as comparative data for future studies. However, we advise caution when interpreting our results, despite achieving statistical significance.

Pd nanoparticles supported on magnetic CoTiMgLDH with enhanced catalytic activity in Suzuki cross‐coupling and reductive degradation of dyes

With an aim to combine the catalytic properties of Pd nanoparticles (NPs) with the excellent characteristics of porous layered double hydroxides (LDH), in the present study, four different catalysts (Pd/Fe3O4‐CoTiMgAlLDH, Pd/Fe3O4‐CoTiMgLDH, Pd/Fe3O4‐CoTiAlLDH and Pd/Fe3O4‐CoTiLDH) were synthesized by supporting Pd NPs onto four different Fe3O4‐LDH supports, which were synthesized by varying the metals in LDH. The catalytic activity of these catalysts was studied for Suzuki coupling and reductive degradation of dyes. Pd/Fe3O4‐CoTiMgLDH outperformed the other catalysts in both reactions. The synthesized catalysts were examined via different characterization techniques like X‐ray diffraction (XRD), Brunauer–Emmett–Teller analysis (BET), X‐ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA), high resolution transmission electron microscopy (HR‐TEM), field emission scanning electron microscopy (FE‐SEM), energy dispersive X‐ray (EDX), energy dispersive X‐ray mapping (SEM–EDX mapping), inductively coupled plasma atomic emission spectroscopy (ICP‐AES) and vibrating sample magnetometry (VSM). On the basis of results obtained from XPS and the experimental data, Fe3O4‐CoTiMgLDH was found to be the support of choice as it not only stabilized the Pd0 NPs but also increased the electron density on the anchored Pd0 species, which enhanced the catalytic activity of Pd/Fe3O4‐CoTiMgLDH for studied organic transformations.

Mathematical Assessment of Combined Standard Uncertainty of Measurements in Using Concentration Ratio Calibration in Inductively Coupled Plasma Atomic Emission Spectrometry

The mathematical assessment of effect of uncertainty components on measurement results in using concentration ratio calibration in inductively coupled plasma atomic emission spectrometry was performed. Formulas for the calculation of the relative standard uncertainty for different components were derived. It was shown that, in different scenarios of using concentration ratio calibration, the combined standard uncertainty basically depends on the repeatability of the determination of the intensity ratio of the analytical line of a test element to the line of the main matrix component of the sample

Determination of the Matrix Composition of Glasses of the Ga–Ge–Te–I System by Inductively Coupled Plasma Atomic Emission Spectrometry

A procedure is developed for the high-precision determination of matrix elements of high-purity glasses of the Ga–Ge–Te–I system, containing from 5 to 15 at % Ga, from 10 to 20 at % Ge, from 69 to 75 at % Te, and from 1 to 6 at % I, using inductively coupled plasma atomic emission spectrometry. The procedure includes two stages independent of each other: determination of the ratio of the mass fractions of Ga and Te to the mass fraction of Ge (stage 1) and determination of the mass fraction of I (stage 2) in the glass sample. Based on these values, the mass and mole fractions of each matrix element of the analyzed sample were calculated. Sample preparation includes the acid dissolution (provides quantitative transfer of Ga, Ge, and Te into the solution) and alkaline opening (provides quantitative transfer of I into the solution) of samples. The accuracy of the results of analysis was confirmed by comparing the results of an analysis of model solutions and model glass samples with the calculated composition. The estimated uncertainty of the results of analysis is 0.05–0.1 at % at P = 0.95.

Mathematical Assessment of Combined Standard Uncertainty of Measurements in Using Concentration Ratio Calibration in Inductively Coupled Plasma Atomic Emission Spectrometry

Mathematical Assessment of Combined Standard Uncertainty of Measurements in Using Concentration Ratio Calibration in Inductively Coupled Plasma Atomic Emission Spectrometry

Determination of the Matrix Composition of Glasses of the Ga–Ge–Te–I System by Inductively Coupled Plasma Atomic Emission Spectrometry

Determination of the Matrix Composition of Glasses of the Ga–Ge–Te–I System by Inductively Coupled Plasma Atomic Emission Spectrometry

Investigating the novel process for thorough removal of eutectic phosphate impurities from phosphogypsum

Phosphogypsum is the major component in solid waste of phosphoric acid manufacturing. After purification, phosphogypsum can be used as an alternative material to natural gypsum. Phosphate impurities, especially eutectic phosphorus, are challenging to be removed thoroughly from phosphogypsum. In this work, we reported a novel phosphogypsum purification process, in which the phase transition activation by calcination was combined with sulfuric acid dissolution during hydration. The two critical parameters, activation temperature and H2SO4 concentration were optimized for this process. Moreover, powder X-ray diffraction (XRD), Fourier transform infrared spectrometer (FTIR), X-ray photoelectron spectrometer (XPS) and inductively coupled plasma atomic emission spectroscopy (ICP-AES) were used to determine the purification efficiency for removing eutectic phosphate impurity from phosphogypsum. The comprehensive characterization results suggested that this novel process can remove eutectic phosphate impurities through the mutual transformation of different crystalline forms of calcium sulfate combined with sulfuric acid dissolution. Under the optimal purification condition (165 °C activation and 1.0 wt% H2SO4), the removal rate of eutectic phosphorus reached up to 98.3%, corresponding to overall eutectic phosphorus content decreasing from 0.58% to 0.01%. Meanwhile, the water-soluble phosphorus and insoluble phosphorus were also completely removed. Thus, 99.4% of phosphate impurity (as P2O5) was removed from phosphogypsum after the two-step treatment. The findings of this paper indicated that this novel process could separate phosphate impurity in an efficient and thorough manner, enabling sustainable utilization of phosphogypsum.

Preliminary Study of Iron Concentration in the Human Placenta in Twin Pregnancies.

Pregnancy significantly increases the demand for iron (Fe) in the female body to facilitate maternal blood volume expansion, placental development, and fetal growth. As Fe flux in pregnancy is significantly influenced by the placenta, the aim of this study was to determine the dependencies between the Fe concentration in the placenta, the infant's morphometric parameters and the woman's morphological blood parameters in the last trimester. The study was conducted on 33 women with multiple (dichorionic-diamniotic) pregnancies from whom the placentas were drawn, and their 66 infants, including pairs of monozygotic (n = 23) and mixed-sex twins (n = 10). Fe concentrations were determined based on inductively coupled plasma atomic emission spectroscopy (ICP-OES) using ICAP 7400 Duo, Thermo Scientific. The results of the analysis showed that lower placental Fe concentrations were associated with deteriorated morphometric parameters of infants, including weight and head circumference. Although we found no statistically significant dependencies between Fe concentration in the placenta and the women's morphological blood parameters, higher Fe concentration in the placenta of mothers supplemented with Fe correlated with better morphometric parameters in infants compared to those whose mothers received no Fe supplementation. The research adds additional knowledge for placental iron-related processes during multiple pregnancies. However, many limitations of the study do not allow detailed conclusions to be assessed, and statistical data should be assessed conservatively.

Composition of the Fluid in Carbonate- and Chlorine-Bearing Pelite near the Second Critical Point: Results of Diamond Trap Experiments

Abstract—The composition of the fluid in carbonate- and chlorine-bearing pelite was experimentally studied at 3.0 GPa and 750 and 900 ºC, using the diamond trap method. The results of inductively coupled plasma atomic-emission spectrometry (ICP AES) and mass balance calculations showed that a supercritical fluid formed in the studied system at 3.0 GPa and 750 °C. The fluid is Si- and Al-rich and contains 30–50 wt.% H2O + CO2 and up to 1 wt.% Cl. The contents of other major elements decrease in the order: K &amp;gt; Na &amp;gt; Сa ≈ Fe &amp;gt; Mg &amp;gt; Mn &amp;gt; Ti ≈ P. Compared with supercritical fluids appeared in the systems pelite–H2O and eclogite–H2O, the fluid with high CO2 and Cl contents is richer in Fe, Ca, Mg, and Mn but poorer in Si. Silicate melt generated in this system at 900 ºС has a composition typical of pelitic melt. Our experiments reveal a set of fingerprints of element fractionation between a supercritical fluid and solids forming an eclogite-like association, namely, high mobility of P, Sr, and B and low mobility of Li and S. Thus, a supercritical fluid compositionally similar to the pelitic melts generated in subduction zones can transfer significant amounts of both volatiles (H2O, CO2, Cl, and P) and major components to the regions of arc magma generation. It is important that supercritical fluids should have trace element signatures of diluted low-temperature fluids.

Chemical Regeneration of Activated Carbon Used in A Water Treatment System for Medical Services

The chemical regeneration of exhausted granular activated carbon (GAC) from a water treatment plant to produce dialysis water used in hemodialysis treatments for chronic renal disease patients from a general Hospital of Ciego de Avila province, Cuba, was investigated. Activated carbon (AC) exhausted mainly by inorganics (Ca (Ca-chelates), Mg and Na) was regenerated using hydrochloric acid and acetic acid (one regeneration cycle). Solutions of 5%, 10%, 15% and 20%(v/v) as well as four contact times (2 h, 4 h, 6 h and 48 h) for hydrochloric acid and three contact times (2 h, 4 h and 6 h) for acetic acid at 25°C and 1 atm in a dosage of 1 g GAC/10 mL were used. Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES), thermogravimetric analysis (TGA), X-ray absorption technique (XRA) and Scanning Electronic Microscopy (SEM) were used to evaluate the effect of the regeneration on exhausted GAC. Batch and scaled column experiments were developed. Breakthrough curves were obtained to assess the AC’s performances after chemical regeneration. The removal/adsorption capacity towards free chlorine (as disinfection agent) and hardness ions (expressed in mg CaCO&lt;sub&gt;3&lt;/sub&gt;/L) was estimated using the area under the breakthrough curves from scaled columns experiments. The hydrochloric acid arises as the best acidic regenerator; using a concentration of 20%(v/v), regenerated GACs using hydrochloric acid showed the highest desorption rate of inorganics as well as a free chlorine removal performance of around 30% concerning the virgin GAC sample. A new GAC management scheme is proposed for GACs used in the medical industry to improve the sustainability and economics of the water treatment process.

Effect of water on the accelerated sulfur vulcanization of natural rubber

Water present in natural rubber was found to play a role in forming carbon-carbon crosslinking junctions before forming carbon-sulfur crosslinking junctions when its effect on the accelerated sulfur vulcanization was investigated by analyzing low–molecular weight products through various instrumental analytical techniques. Samples were prepared by mixing deproteinized natural rubber (DPNR) with various moisture contents with stearic acid, ZnO, sulfur, and N-tert-butylbenzothiazole-2-sulfenamide, and they were vulcanized at 150 °C for various cure times. Low–molecular weight products such as 2,2′-dibenzothiazole disulfide (MBTS), 2-mercaptobenzothiazole (MBT), ZnMBT, Zn2+ and sulfur linked to the rubber were extracted from the vulcanized natural rubbers using benzene and dioxane, and subsequently measured by high-performance liquid chromatography, UV–visible spectroscopy, inductively coupled plasma atomic emission spectroscopy, and combustion analysis. The water present in natural rubber was found to strongly affect the production and formation rate of the low–molecular weight products in the accelerated sulfur vulcanization of natural rubber. As the result it suggests that the water promotes the formation of the C-C linkages, and then it sequentially promotes the formation of the C-S linkages.

NMR-Relaxometric Investigation of Mn(II)-Doped Polyoxometalates in Aqueous Solutions.

Solution behavior of K;5[(Mn(H2O))PW11O39]·7H2O (1), Na3.66(NH4)4.74H3.1[(MnII(H2O))2.75(WO(H2O))0.25(α-B-SbW9O33)2]·27H2O (2), and Na4.6H3.4[(MnII(H2O)3)2(WO2)2(β-B-TeW9O33)2]·19H2O (3) was studied with NMR-relaxometry and HPLC-ICP-AES (High Performance Liquid Chromatography coupled with Inductively Coupled Plasma Atomic Emission Spectroscopy). According to the data, the [(Mn(H2O))PW11O39]5- Keggin-type anion is the most stable in water among the tested complexes, even in the presence of ethylenediaminetetraacetic acid (EDTA) or diethylenetriaminepentaacetic acid (DTPA). Aqueous solutions of 2 and 3 anions are less stable and contain other species resulting from dissociation of Mn2+. Quantum chemical calculations show the change in Mn2+ electronic state between [Mn(H2O)6]2+ and [(Mn(H2O))PW11O39]5-.

Preparation of Zinc Nanoparticles by Gas Condensation in a Contactless Crucible

In this work, zinc nanoparticles were obtained. As a production method, a one-stage induction flow levitation method was used. The starting material was spherical granules with a purity of 99.9% and a mass of 2 g; as atoms evaporated from the surface of the molten granule, the drop was fed with a metal wire made of the same material. The productivity of the nanoparticles was 30 g / h. The resulting nanoparticles were characterized by scanning electron microscopy, X-ray phase analysis, porosimetry, and inductively coupled plasma atomic emission spectroscopy.

ONTOGENETIC FEATURES OF THE ELEMENTAL COMPOSITION OF DOG HAIR

This work aims to study the elemental status of dog hair in ontogeny. The studies were conducted on animals 2–4 and 8–10 years of age. Under observation were 39 dogs of the following breeds: Rottweilers, Dalmatians, Black Terriers, Golden Retrievers, Labradors and Dobermans. The animals were born and kept in Novosibirsk, Tomsk, Yalta and Moscow. The dogs were kept in apartments with obligatory morning and evening exercise. Wool was sheared from the withers to determine the concentration of bioelements. The bioelemental composition of wool was determined on an Elan 9000 quadrupole mass spectrometer and an Optima 2000DV atomic emission spectrometer by inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry. The research was carried out during the summer period. The diet of dogs consisted of dry industrial feed, balanced in terms of essential nutrients, vitamins, and macro- and microelements. In the research process, specific microelementoses were found in dogs of different ages. The obtained results showed that dogs of 2-4 years of age exceed 8-10-year-old animals in the concentration of aluminium in wool by 81.3% (P&lt;0.01), chromium - by 67.1 (P&lt;0.001), copper - by 27.4 (P&lt;0.05), iron - by 81.7 (P&lt;0.05), mercury - by 70.5 (P&lt;0.05), iodine - by 68.3 (P&lt; 0.05), potassium – by 57.5 (P&lt;0.01), lithium – by 65.7 (P&lt;0.05), lead – by 84.5 (P&lt;0.05), vanadium – by 56.6 (P&lt;0.05) and zinc by 27.9% (P&lt;0.01). At the same time, in the group of 2-4-year-old animals, the iodine level exceeded the limit of reference values by 35.5%. On the other hand, in dogs of 8–10 years, chromium, iron, iodine, manganese, and silicon indicators have lagged behind the lower limit of the reference values by 45.0, respectively; 89.9, 86.0, 91.0 and 89.7%.