Inductively Coupled Plasma-atomic Emission Spectroscopy Analysis Research Articles

Development of Cu application using dual-energy computed tomography for detecting medication-related osteonecrosis of the jaw.

The present study developed an application using dual-energy computed tomography (DECT) focused on Cu for detecting medication-related osteonecrosis of the jaw (MRONJ). First, we performed two types of phantom studies using a Cu wire syringe and pig mandible with Cu wire to detect Cu on DECT. Second, DECT examinations of 44 patients with MRONJ were performed to compare lesion and normal bone sites using single-energy CT, DECT-virtual non-calcium (VNCa), and DECT-Cu applications. Quantitative analyses of VNCa CT and CT values were performed, and a cut-off value was calculated using receiver operating characteristic analysis. Third, we compared the Cu content in the MRONJ and normal bone groups using inductively coupled plasma atomic emission spectroscopy (ICP-AES). The material-specific differences in attenuation between the two different energies enabled the accurate separation of Cu from Ca in phantom studies. The sensitivity and specificity for single-energy CT, DECT-VNCa, and DECT-Cu applications were 97.7% and 2.3%, 86.4% and 81.8%, and 88.6% and 97.7%, respectively. Thus, VNCa CT values obtained on DECT-Cu application images showed the highest area under the curve value and maximal diagnostic efficacy in differentiating lesion sites from normal bone sites. On ICP-AES analyses, the Cu content was significantly higher in the MRONJ group than in the normal bone group. DECT-Cu application demonstrated better diagnostic performance in detecting MRONJ compared with single-energy CT or DECT-VNCa.

Construction of a Stimuli-Responsive DNAzyme-Braked DNA Nanomachine for the Amplified Imaging of miRNAs in Living Cells and Mice

Construction of a Stimuli-Responsive DNAzyme-Braked DNA Nanomachine for the Amplified Imaging of miRNAs in Living Cells and Mice

Atomically Dispersed Manganese Lewis Acid Sites Catalyze Electrohydrogenation of Nitrogen to Ammonia

Atomically Dispersed Manganese Lewis Acid Sites Catalyze Electrohydrogenation of Nitrogen to Ammonia

Comparative pharmaceutico-analytical study of Rasamanikya prepared by two different Shodhana media of Haratala (orpiment).

Introduction:Foremost, Rasamanikya is described in Rasendra Chintamani by Acharya Dhundhuknath. It is a formulation that is prepared from the arsenical drug, i.e., orpiment (Haratala). Haratala is classified under Uparasa Varga in Rasa classics and is also included under Schedule E1 in D and C act 1940. In classics, there are so many media mentioned for purification process (Shodhana) of orpiment. In the present study, Kushmanda Swarasa (juice of Benincasa hispida [Thunb.] Cogn) and Churnodaka (lime water) are adopted as the purification media for orpiment.Aim:The aim of this study was to standardize the pharmaceutical procedure of Rasamanikya and develop a comparative analytical profile of both the formulation, i.e., Rasamanikya prepared by Kushmanda Swarasa and Churnodaka Shodhita Haratala.Materials and methods:The study was carried out in two stages as follows: Shodhana of Haratala and preparation of Rasamanikya by Kupipakwa method. Both the samples of Rasamanikya were analyzed for organoleptic and physicochemical parameters. The samples of final products were also analyzed through sophisticated analytical parameters, i.e., X-ray diffraction (XRD), Inductively coupled plasma-atomic emission spectroscopy (ICP-AES), CHNS and O, Field emission gun-scanning electron microscopy (FEG-SEM), Fourier transform infrared spectroscopy (FTIR) and Thermo-gravimetric analysis (TGA).Results:Average 2 h duration was required for the preparation of Rasamanikya formulation from 600 g of purified orpiment. In XRD analysis, both samples have different diffraction patterns. In ICP-AES analysis, both samples have the same percentage of arsenic. More percentage loss was noted in the TGA of Rasamanikya prepared with Churnodaka Shodhita Haratala than that of Kushmanda Swarasa Shodhita Haratala.Conclusion:Rasamanikya prepared by two different media of Shodhita Haratala did not found to have a substantial difference in pharmaceutical procedure. However, there was a considerable difference in the analytical study. Kupipakwa procedure can be used for large-scale preparation.

Aqueous solution growth at 200 °C and characterizations of pure, 17O- or D-based herbertsmithite ZnxCu4-x(OH)6Cl2 single crystals

Abstract The aqueous solution growth of mm-sized, pure, 17O- or D-enriched herbertsmithite ZnxCu4-x(OH)6Cl2 single crystals is presented. A relationship between x values, antisite disorder amounts and the growth temperature is established. The crystal chemical composition and stability, structural phase and antisite disorder amounts have been characterized by powder X-ray diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS), Electron Probe Micro Analysis/Wavelength Dispersive Spectroscopy (EPMA/WDS), Inductively Coupled Plasma/Atomic Emission Spectroscopy analysis (ICP/AES), coupled Thermo Gravimetric Analysis-Mass Spectrometry (TGA/MS) and magnetic susceptibility measurements. An unambiguous relationship between the c lattice parameter and the x value has been found.

Quantitation and distribution of metallic elements in sequestra of medication-related osteonecrosis of jaw (MRONJ) using inductively coupled plasma atomic emission spectroscopy and synchrotron radiation X-ray fluorescence analysis.

Medication-related osteonecrosis of the jaw (MRONJ) is a serious adverse effect of antiresorptive agents like bisphosphonates. Abnormal concentrations of various trace metallic elements contained in bone minerals have been associated with MRONJ. In this study, we focused on trace metallic elements contained in the MRONJ sequestrum; their content and distribution were compared to those in osteomyelitis and non-inflammatory bones using inductively coupled plasma atomic emission spectroscopy (ICP-AES) and synchrotron radiation X-ray fluorescence analysis (SR-XRF). On ICP-AES analyses, various trace elements (Co, Cr, Cu, Fe, K, Mg, Ni, Sb, Ti, V, Pb) were significantly more in MRONJ sequestra than non-inflammatory bones. The Cu content was significantly higher in MRONJ sequestra than osteomyelitis and non-inflammatory bones. The Cu content in MRONJ sequestra was high even after decalcification. Additionally, Cu was distributed along the trabecular structures in decalcified MRONJ specimens, as observed using SR-XRF analysis. Therefore, this study was indicative of the characteristic behavior of Cu in MRONJ.

Ce@STANPs/ZrO2 as Nanocatalyst for Multicomponent Synthesis of Isatin-Derived Imidazoles under Green Reaction Conditions.

A highly efficient and recyclable catalyst, cerium-immobilized silicotungstic acid nanoparticle-impregnated zirconia (Ce@STANPs/ZrO2), has been synthesized. The catalytic activity of Ce@STANPs/ZrO2 was investigated for the first time in multicomponent synthesis of isatin-based imidazoles under microwave irradiation in water. Ce@STANPs/ZrO2 was used for C=O bond activation in overall reaction to synthesize isatin-based imidazoles. The structure of catalyst was confirmed by characterization techniques, such as Fourier transform infrared (FTIR), scanning electron microscopy (SEM)/energy dispersive X-ray, elemental mapping, transmission electron microscopy, ζ-potential and diffraction light scattering, X-ray diffraction (XRD), thermogravimetric analysis, temperature-programmed desorption-NH3, electron paramagnetic resonance (EPR), and inductively coupled plasma atomic emission spectroscopy (ICP-AES) analyses. The recovered catalyst was found to be efficient up to seventh cycle and was confirmed by FTIR, SEM, XRD, EPR, and ICP-AES analyses. The advantages of the present protocol are recyclability of catalyst, green reaction conditions, excellent yield (94%) of the products, shorter reaction time period (5–7 min), and clean reaction profile.

Poly(tetrafluoroethylene)-Stabilized Metal Nanoparticles: Preparation and Evaluation of Catalytic Activity for Suzuki, Heck, and Arene Hydrogenation in Water.

Poly(tetrafluoroethylene)-stabilized Pd nanoparticles (PTFE-PdNPs) were prepared in water with 4-methylphenylboronic acid as a reductant and characterized using powder X-ray diffraction, transmission electron microscopy (TEM), X-ray photoelectron spectroscopy, and inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Small PdNPs with a fairly uniform size were obtained in the presence of PTFE, whereas aggregation of palladium was observed in the absence of PTFE. PTFE-PdNPs showed high catalytic activity for the Suzuki coupling reaction in water and were reused without any loss of activity. No palladium species were observed by ICP-AES analysis in the reaction solution after the reaction, nor was any change in particle size observed after the recycle experiment. PTFE-PdNPs also exhibited excellent catalytic activity and reusability for the Heck reaction in water. Although palladium species were not detected in the reaction solution after the reaction, aggregates and smaller sizes of PdNPs were observed in the TEM image of the recovered catalyst. PTFE was also useful as the stabilizer of rhodium nanoparticles (RhNPs) prepared by reduction with NaBH4. PTFE-RhNPs showed high catalytic activity and reusability toward arene hydrogenation under mild conditions.

Polyoxometalate intercalated layered silicates: Highly efficient catalytic epoxidation of cyclooctene

Polyoxometalates (POMs) are a class of discrete anionic metal oxides with unique physical and chemical properties. Owing to excellent redox activity and structural adjustability, POMs-based catalysts have drawn wide attention during past decades. However, homogenous POMs exhibit high crystallinity behavior, which result in aggregation and/or recycling difficulty. Therefore, appropriate supports are highly needed to achieve well dispersion and stable loading of POMs on supports. Layered silicates are a large family of two-dimensionally arranged cation-exchangeable layered materials, whose frameworks are composed of SiO4 tetrahedral and possess interlayer exchangeable cations that are often hydrated. Most importantly and interestingly, layered silicates can turn to be anion exchangeable materials through covalent modification of imidazolium salts containing terminal triethoxysilyl groups onto interlayer surface. As a result, layered silicates can generate a large variety of interesting structures and properties. Among them, the layered octosilicate (Na8Si32O64(OH)8·32H2O, Oct) is an ideal support due to its optimal arrangement and high density of SiOH/SiO−. It is worthwhile noting that more than 80% of interlayered SiOH/SiO− groups can be silylated with imidazolium salts generally, and are converted to anion exchangeable sites. Herein, the ionic liquid modified layered silicates (IL-Oct) have been synthesized through immobilization of 1-octyl-3-(3-triethoxysilylpropyl)-4,5-dihydroimidazolium-hexafluorophosphate (Oim-PF6) on the interlayered surface of layered silicates. The cation exchangeable sites on layered silicates can be stoichiometrically converted to anion exchangeable sites after modification. Further ion exchange with K7PW11O39·12H2O (PW11), we are able to successfully fabricate the POM-intercalated layered silicates material that can be denoted as PW11-IL-Oct. The resulting PW11-IL-Oct has been fully characterized using a variety of spectroscopy methods including X-ray diffraction (XRD), scanning electron microscope (SEM), high resolution transmission electron microscopy (HRTEM), Brunauer-Emmett-Teller (BET) gas adsorption method, inductively coupled plasma-atomic emission spectroscopy (ICP-AES) and energy dispersive spectrometer (EDS), etc. XRD pattern of PW11-IL-Oct reveals the basal spacing of 2.85 nm. The calculated gallery height value is 2.11 nm by subtracting the thickness of the host layer (0.74 nm). The BET surface areas of IL-Oct and PW11-IL-Oct are 5.7 and 15.4 m2/g, respectively. The loading amount of PW11 in PW11-IL-Oct is 7.34wt% by ICP-AES analysis. SEM images of PW11-IL-Oct show the square plate morphology with distortion and wrinkles on the surface. The SEM Mapping results suggest that the POMs clusters are highly dispersed and orderly arranged in the two-dimensional (2D) confined gallery spaces. Moreover, HRTEM images and EDS result of the PW11-IL-Oct reveal the highly dispersed black spots with the diameter approximately ~1 nm, which is in good agreement with the particle size of PW11 clusters. Epoxides are widely utilized as raw materials for sythesis of biologically important pharmaceuticals and fine chemicals. The application of epoxides is growing fast in the chemical industry, and gives rise to remarkable attention within the scientific community. In this work, by using the expoxidation of cyclooctene as model reaction, we demostrate that the PW11-IL-Oct exhibits excellent activity and stablity. The yield of epoxides product reaches up to 98% in 1 h with >99% selectivity. Moreover, after 10 recycles, no obvious loss of activity can be observed and the loading amount of PW11 in PW11-IL-Oct maintain 7.16wt%. HRTEM and Mapping results show almost no aggreaction of PW11 clusters in the layered silicates after epoxidation reaction. This work paves a pathway for fabrication of novel POMs-based catalysts.

Exploration of Novel Oxide Cathode Materials for Proton-Conducting Solid Oxide Fuel Cell: Phase Relation in the Ba(Zr, Y)O3-Ba(Co, Y)O3-Ba(Fe, Y)O3 System

1. Introduction Proton-conducting solid oxide fuel cell (pc-SOFC) is expected to be one of the most efficient, highly stable, and cost-effective SOFC. As a cathode material for pc-SOFC, a composite cathode system, which comprises of both electron- and proton-conducting materials, has been examined and developed. In such cases, reaction area is limited to the triple phase boundary (TPB), and resultant cathode performance is poor in most cases. On the other hand, upon successful development of mixed proton-hole conductor (MphC) for the oxide cathode, the reaction area will be expanded to the whole surface of cathode grains, because the reaction area turned into two-dimensional boundary from one-dimensional TPB, and the efficiency of the cell will be significantly enhanced[1]. Our primary strategy to develop protonic/electronic mixed conductor for a pc-SOFC cathode is to realize a double percolation system in a single phase of solid solution, that is, Y-doped BaZrO3 (BZO) as a proton conducting host matrix, doped with Co and Fe for the formation of percolation network of electronic carriers, since BaZrO3 is reported as chemically stable perovskite with the best proton conductivity at the target temperature between 400 to 600 °C[2]. In addition, the electronic conductivity is reported in Co-[3] or Fe-doped[4] BaZrO3, while a possible low solubility of Co and its poor chemical stability has to be resolved. Fe is known to dissolve to form solid solution over the entire composition range in the BZO-BaFeO3 quasi binary system at elevated temperatures, providing both chemical stability and the hole conductivity to BZO. As the first step of the development of the MphC cathode materials, phase relation in the Ba(Zr, Y)O3-Ba(Co, Y)O3-Ba(Fe, Y)O3 system at elevated temperatures is examined to understand the feasibility of the present system to the double percolation scheme. In this study, the composition is expressed as BCFZYxyz1 for the formula, BaCox/10Fey/10Zrz/10Y0.1O3-δ, and BCFZY4411, corresponding to the composition of novel cathode for pc-SOFC reported by Duan et al.[5], is included in this compositional contour of the present study. Also further analyses including electrical conductivity and so on will be reported. 2. Experimental Powders of BaCox/10Fey/10Zr0.9-x/10-y/10Y0.1O3-δ with x and y ranging from zero to nine were synthesized via the Pechini method from nitrate aqueous solutions. Concentrations of cations in the nitrate aqueous solutions were determined by both chemical titration and an inductively coupled plasma atomic emission spectroscopy (ICP-AES). The powders were calcined at 1000 °C for 2 h, pressed into pellets using a uniaxial pressing at 1000 kgf/cm2 with an 11.3 mm diameter mold, and subsequently sintered for 10 h at either 1200, 1300, or 1400 °C. The pellets were ground into powders and X-ray diffraction (XRD) measurements were performed with the obtained powders. A field emission scanning electron microscopy and (FESEM) and an energy dispersive X-ray spectroscopy (EDX) were performed on the polished fresh surfaces of the pellets and the annealed surfaces of the pellets after thermal etching. 3. Results and Discussion From the results of XRD measurements, the most of the peaks observed in the XRD patterns were attributed to the primary cubic perovskite structure in reference to the ICDD data for cubic BaZrO3. In BCFZY3061, 3151, 3241, 3331, 2251, and 1351, peaks from the secondary perovskite phase were observed, while those from secondary and tertiary perovskite phases were observed in BCFZY4411 and 4141. The secondary and tertiary phases, however, were not clearly identified by EDX. In most of the samples, the peaks indexed with BaCO3 were observed because of the BaO-rich composition of the precursors identified by ICP-AES analyses. The other peaks were attributed to the impurity phases such as BaCoO3 and YBaCo4O7. In BCFZY3061, 3151, 3241, 3331, 4411, and 4141, partially melted area and thin plate-/needle-like crystals were observed with FESEM. These crystals were identified as YBaCo4O7 or its analog from the EDX results. In addition to the EDX analyses, from the relation between lattice constants of cubic BaZrO3-like phases and Fe/(Co+Fe+Zr) ratio, the phase relation in the BaZr0.9Y0.1O3-δ-BaFe0.9Y0.1O3-δ-BaCo0.9Y0.1O3-δ quasi-ternary system is estimated and proposed that there exist four separate solid solutions of BaZrO3-, BaFeO3-, BaCoO3- based phases and an intermediate phase between Ba(Zr, Co)Y0.1O3 and Ba(Zr, Fe)Y0.1O3.

Effects of surface friction treatment on the in vitro release of constituent metals from the biomedical Co–29Cr–6Mo–0.16N alloy

Due to the ignorance by many researchers on the influence of starting microstructure on the metal release of biomedical materials in human body after implant, in this study, the effect of surface friction treatment on the in vitro release of the constituent elements of the biomedical Co–29Cr–6Mo–0.16N (CCM) alloy is investigated for the first time by immersion test in lactic acid solution combined with electron backscatter diffraction, transmission electron microscope, X-ray diffraction, X-ray photoelectron spectroscopy, and inductively coupled plasma atomic emission spectroscopy (ICP-EOS). The results indicate that friction treatment on the as-annealed CCM alloy sample surface leads to a planar strain-induced martensitic transformation (SIMT) on sample surface; this greatly accelerates the release of all the constituent elements and, in particular, that of Co as indicated by the ICP-EOS analysis. This increase can be ascribed to a localized deformation that occurred over the entire sample surface, with the dislocation density being high within the SIMTed phase and low in the alloy matrix.

Evaluation of the toxic potential of calcium carbide in the third instar larvae of transgenic Drosophila melanogaster (hsp70-lacZ)Bg9

In the present study the toxic potential of calcium carbide (CaC2) was studied on the third instar larvae of transgenic Drosophila melanogaster (hsp70-lacZ)Bg9. The third instar larvae were exposed to 2, 4, 8, 16 and 32×10−3g/ml of CaC2 in diet for 24h. The results reveal that the dose 2×10−3g/ml was not toxic but the remaining doses showed a dose dependent significant increase in the hsp70 expression, β-galactosidase activity, tissue damage, oxidative stress markers (lipid peroxidation and protein carbonyl content), glutathione-S-transferase activity, expression of Caspase 3 and 9, apoptotic index and DNA damage (midgut cells). A significant reduction as compared to control group in total protein, glutathione content and acetylcholinesterase activity was also observed. The Inductively Coupled Plasma Atomic Emission Spectroscopy analysis (ICPAES) reveals the presence of copper, iron, sodium, aluminium, manganese, calcium, nickel and mercury. The toxic effects of CaC2 in the present study may be attributed to the impurities present in it.

Fostering hydroxyapatite bioactivity and mechanical strength by Si-doping and reinforcing with multiwall carbon nanotubes.

The aim of the present study was to prepare resorbable hydroxyapatite (HA) based bone graft materials reinforced with carbon nanotubes as a way to cope with the inability of pure HA to resorb and its intrinsic brittleness and poor strength that restrict its clinical applications under load-bearing conditions. With this purpose, a Si-doped HA nanopowder (n-Si0.8HA) was prepared by chemical synthesis and used as composite matrix reinforced with different amounts of functionalized multiwall carbon nanotubes (MWCNTs). The effect of the added amounts of MWCNTs on the mechanical properties of nanocomposites and their in vitro biomineralization was assessed by bending strength measurements, immersing tests in simulated body fluid solution (SBF), scanning electron microscopy (SEM), and inductively coupled plasma atomic emission spectroscopy analysis (ICP-AES). The bioactivity and bending strength were enhanced, reaching maximum balanced values for an optimum addition of 3 wt.% f-MWCNTs. These results might contribute to broaden the potential applications of HA-based bone grafts.

Welding fumes from stainless steel gas metal arc processes contain multiple manganese chemical species

Fumes from a group of gas metal arc welding (GMAW) processes used on stainless steel were generated using three different metal transfer modes and four different shield gases. The objective was to identify and measure manganese (Mn) species in the fumes, and identify processes that are minimal generators of Mn species. The robotic welding system was operated in short-circuit (SC) mode (Ar/CO2 and He/Ar), axial spray (AXS) mode (Ar/O2 and Ar/CO2), and pulsed axial-spray (PAXS) mode (Ar/O2). The fumes were analyzed for Mn by a sequential extraction process followed by inductively coupled plasma-atomic emission spectroscopy (ICP-AES) analysis, and by X-ray diffraction (XRD). Total elemental Mn, iron (Fe), chromium (Cr) and nickel (Ni) were separately measured after aqua regia digestion and ICP-AES analysis. Soluble Mn2+, Fe2+, Fe3+, and Ni2+ in a simple biological buffer (phosphate-buffered saline) were determined at pH 7.2 and 5.0 after 2 h incubation at 37 C by ion chromatography. Results indicate that Mn was present in soluble form, acid-soluble form, and acid-soluble form after reduction by hydroxylamine, which represents soluble Mn0 and Mn2+ compounds, other Mn2+ compounds, and (Mn3+ and Mn4+) compounds, respectively. The dominant fraction was the acid-soluble Mn2+ fraction, but results varied with the process and shield gas. Soluble Mn mass percent in the fume ranged from 0.2 to 0.9%, acid-soluble Mn2+ compounds ranged from 2.6 to 9.3%, and acid plus reducing agent-soluble (Mn3+ and Mn4+) compounds ranged from 0.6 to 5.1%. Total Mn composition ranged from 7 to 15%. XRD results showed fumes had a crystalline content of 90-99% Fe3O4, and showed evidence of multiple Mn oxides, but overlaps and weak signals limited identification. Small amounts of the Mn2+ in the fume (<0.01 to ≈ 1% or <0.1 to ≈ 10 microg ml(-1)) and Ni2+ (<0.01 to ≈ 0.2% or <0.1 to ≈ 2 mg ml(-1)) ions were found in biological buffer media, but amounts were highly dependent on pH and the welding process. Mn generation rates for the fractions were tabulated, and the influence of ozone is discussed. The conclusions are that exposures to welding fumes include multiple Mn species, both soluble and insoluble, and that exposures to Mn species vary with specific processes and shield gases.

Synthesis and Characterization of NiO-8YSZ Powders by Coprecipitation Route

Nickel oxide – 8 mol% yttria stabilized zirconia (NiO-8YSZ) powders containing 25 to 75 wt% of NiO were prepared by coprecipitation. The entire process includes the reaction of metals aqueous chloride solutions (heated at 95 oC) with ammonium hydroxide, washing steps of the resulting gel, butanol azeotropic distillation treatment to prevent the formation of hard agglomerates, drying, calcination and ball milling. The yield of precipitation of metals was determined by inductively coupled plasma atomic emission spectroscopy analysis (ICP-AES). Powders were characterized by X-ray and laser diffraction, infrared analysis, gas adsorption (BET) and scanning electron microscopy. It was observed that zirconium and yttrium hydroxides are easily precipitated in alkaline medium, while nickel precipitation yield is in the range of 80 to 95% due to the formation of soluble complexes. NiO appears as a second phase in synthesized powders and contributes to decreasing of specific surface area and agglomerate mean size.

Preparation and evaluation of zirconia microspheres as inorganic exchanger in adsorption of copper and nickel ions and as catalyst in hydrogen production from bioethanol

Abstract In this work, the preparation and performance of a zirconia microspheres inorganic exchanger in uptake of nickel and copper ammoniacal solution is showed. The yield of retention of the metallic ions was determined by inductively coupled plasma atomic emission spectroscopy analysis (ICP-AES). Microspheres were characterized by X-ray diffraction (XRD), gas adsorption (BET). The catalyst of 6%Ni/3%Cu/ZrO2 exhibits high activity for ethanol steam reforming with conversion of ethanol of 100% and selectivity of hydrogen of 60% at 550 °C.