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11.
Lenka Husáková Iva Urbanová Tereza Šídová Michaela Šafránková 《Journal of Analytical Chemistry》2018,73(7):650-660
A method for simultaneous multi-element analysis of fly ash samples by inductively coupled plasma orthogonal acceleration time-of-flight mass spectrometry (oaTOF-ICP-MS) after closed-vessel microwave extraction with ammonium fluoride was introduced here. Corrosive and/or toxic acids like HF, HCl or HClO4, as well as HNO3, which are commonly used during sample preparation of the fly ash samples, are avoided in this method. The spectral effects due to the formation of different Cl, Na, K, Ca, Mg-containing polyatomic species interfering with the determination of a number of elements like As, Se or Ni during the oaTOF-ICP-MS analysis are negligible. Under the optimum experimental extraction conditions evaluated using a fractional factorial design (10 mg of the sample extracted with 5 mL of 140 g/L NH4F for 10 min at 200°C), analysis of the resulting supernatant with Rh as an internal standard enabled precise and accurate simultaneous determination of 11 elements (Li, Be, Ni, As, Se, Rb, Sb, Cs, W, Tl and U) at trace and ultratrace levels. The accuracy was assessed by analysing two certified reference materials, namely Fine Fly Ash CTA-FFA-1 and Constituent Elements in Coal Fly Ash Standard Reference Material® 1633b. The precision of the reported method was better than 10%. 相似文献
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František Kačík Jana Luptáková Pavel Šmíra Adriana Eštoková Danica Kačíková Andrea Nasswettrová Tatiana Bubeníková 《Journal of Thermal Analysis and Calorimetry》2017,128(2):755-764
Glasses having composition 5Li2O–5ZnO– xBi2O3 –(90 ? x) P2O5 (x = 5, 10, 15, 20 and 25 mol%) were prepared by the normal melt quenching technique. Nanocomposite glass containing bismuth phosphate BiPO4 nanocrystals was obtained, which can be attributed to homogeneous nucleation process. The formation of BiPO4 nanocrystals was confirmed and characterized by X-ray diffraction patterns (XRD), transmission electron microscopy (TEM), differential scanning calorimetry, optical absorption (UV–Vis) and micro-hardness studies. The morphological analysis by XRD and TEM microscopy showed the formation of hexagonal BiPO4 nanocrystals, and its estimated nanocrystalline sizes were found to be varying from 5.35 to 11.53 nm depending on the Bi2O3 concentrations. The density (ρ) and molar volume (V m) were also determined and found to be in compositional dependence. Glass transition temperature (T g) and glass crystallization temperature (T c) were obtained and found to be increased (from 240.0 to 337.2 °C) with increasing Bi2O3 up to 20 mol% and then decreased (from 337.2 to 331.8 °C) due to the structural changes in the glass network. Effect of BiPO4 content on the optical properties had been investigated. From the UV–Vis spectra, it was observed that the fundamental absorption edge shifts toward lower wavelengths, i.e., blueshifts with increasing Bi2O3 mol% up to 20 mol%, and then shifts toward higher wavelengths, i.e., redshifts beyond 20 mol%. It was also observed that the obtained E opt (for indirect and direct transitions) increases with gradual increase in Bi2O3 content up to 20 mol% and then decreases beyond 20 mol%. This may be due to the introduction of Bi cations into the glass network as a network former up to 20 mol% causing a decrease in ΔE values, beyond 20 mol%, the introduction of Bi ions into the glass network interstitially leads to increase the values of ΔE. The optical properties of the present nanocrystallized glasses showed a quantum size dependence, in which the optical band gap energy (E opt) was changed as a function of BiPO4 nanocrystalline sizes. 相似文献
14.
Jaromíra Chýlková Markéta Tomášková Lenka Janíková Renáta Šelešovská Tomáš Navrátil Petra Chudobová 《Chemical Papers》2017,71(6):1047-1054
A sensitive voltammetric method for the determination of pyrogallol (PY) was developed employing a boron-doped diamond electrode (BDDE). The composition of the supporting electrolyte was investigated during the development of the methodology. Linear sweep voltammetry (LSV) under the optimized experimental conditions was applied for PY determination with a limit of detection and limit of quantification of 0.85 and 2.82 μmol L?1, respectively. These values are satisfactory for application to real samples. The usability of this method for the quantification of pyrogallol was in range from 2.82 to 296.00 μmol L?1. Finally, the developed method was successfully used for the analysis of real samples of biodiesel produced from rapeseed oil and its blend with diesel fuel. Samples of biodiesel and biodiesel blends were analyzed directly in an electrochemical cell, while samples with very low concentrations of PY in biodiesel were extracted with water using the proposed simple and fast process. 相似文献
15.
In this paper we study some mappings of skew ruled surfaces in simply isotropic space which preserve the generators. We study isometries, conformal mappings and mappings which preserve the area. Furthermore, we study mappings of surfaces in I
3
1 which preserve the asymptotic lines.Received December 18, 2001; in revised form July 12, 2002
Published online April 4, 2003 相似文献
16.
Václav Štengl Snejana Bakardjieva Natalie Murafa Eva Večerníková Jan Šubrt Vladimír Balek 《Journal of nanoparticle research》2007,9(3):455-470
A new method for preparation of titania nanowires with diameter around 10 nm and length up to 2–3 μm is described. The precursor
was prepared from sodium titanate by adding ethylene glycole (EG) and heating at temperature of 198°C for 6 h under reflux.
The sodium titanate glycolate formed by this way aggregated into 1D nanostructures and was subsequently transformed into titania
glycolate during a chemical treatment with 98% sulfuric acid. Titania nanowires with variable amount of anatase and rutile
were prepared by heating to temperatures in the range 350–1000°C. The precursor as well as titania based samples were characterized
by X-ray diffraction, Infrared spectroscopy, Scanning electron microscopy, High resolution transmission microscopy, Thermogravimetry,
Differential thermal analysis, Evolved gas analysis and Emanation thermal analysis. The nitrogen adsorption/desorption was
used for surface area and porosity determination. The photoactivity of the prepared titania samples was assessed by the photocatalytic
decomposition of 4-chlorophenol in an aqueous slurry under UV irradiation of 365 nm wavelength. 相似文献
17.
The Pd-catalysed conjugate addition of arylboronic acids to α,β-unsaturated cyclic ketones was studied under controlled microwave irradiation conditions. A variety of catalysts, bases and
solvents was explored in order to achieve optimum yields in the shortest possible reaction time. Under optimised conditions
(Pd(OAc)2/2,2′-bipyridine and KF in a mixture of toluene, water, and acetic acid and 10 min microwave irradiation), a range of arylboronic
acids was successfully added to several cyclic enones. With chiral phosphane ligands, a promising enantioselectivity was obtained
(85 % ee). 相似文献
18.
Stanislav Šabata Jiří Hetflejš Renata Rychtáriková Gabriela Kuncová Kamil Lang Pavel Kubát 《Chemical Papers》2009,63(4):438-444
Three tetracationic porphyrins differing in the position of charged nitrogen atoms on the peripheral substituents — 5,10,15,20-tetrakis(N-methylpyridinium-4-yl)porphyrin (TMPyP4), 5,10,15,20-tetrakis(N-methylpyridinium-2-yl)porphyrin (TMPyP2), 5,10,15,20-tetrakis(4-trimethylammoniophenyl) porphyrin (TMAPP), and hydrophobic 5,10,15,20-tetraphenylporphyrin (TPP), were immobilized by adsorption
and encapsulation in poly(hydroxymethylsiloxane) (PHOMS). The so prepared porphyrin-PHOMS composites were characterized by
porosimetry, scanning electron microscopy, fluorescence and diffuse reflectance UV-VIS spectroscopy. It was found that porphyrins
are immobilized in the PHOMS matrix in the free base monomer form Their irradiation produced singlet oxygen O2(1Δg) with the lifetime of 10–30 μs. 相似文献
19.
Jolanta Rousseau Vilija Kriščiūnienė Ilona Rimkevičiūtė Cyril Rousseau Virginė Amankavičienė Algirdas Šačkus Arnaud Tatibouët Patrick Rollin 《Monatshefte für Chemie / Chemical Monthly》2009,140(3):339-348
Abstract Modular conditions for the formation of thioureas or pyrimidine-4-one-2-thiones connected to the benzo[b]thiophene, benzene and indole structures were performed. A benzo[b]thiophene isothiocyanate derivative was used as a model to study the condensation with simple aromatic amines and amino-l-sorbose derivative. The construction of pyrimidine-4-one-2-thiones using basic conditions afforded efficiently new heterocyclic
aromatics, which were further transformed using the alkylated sulfur as a leaving group in palladium-catalyzed cross-coupling
reactions.
Graphical abstract
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