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91.
A novel, simple and environmentally friendly procedure for copper determination has been developed. The method is based on the formation of an ion associate of Cu(I) with 1,3,3-trimethyl-2-[5-(1,3,3-trimethyl-1,3-dihydroindol-2-ylidene)-penta-1,3-dienyl]-3H-indolium (DIDC) in the presence of chloride ions as ligand, followed by dispersive liquid-liquid microextraction (DLLME) of the formed ion associate into organic phase and UV-Vis spectrophotometric detection. The following experimental conditions were used: pH 3, 0.24 mol L− 1 chloride ions, 0.06 mmol L− 1 DIDC. The effect of the nature of the extraction solvent, auxiliary solvent and disperser solvent used was studied. A mixture of amyl acetate, tetrachloromethane, and methanol in a 1:1:3 v/v/v ratio was selected for the DLLME procedure. The absorbance of the coloured extracts at 640 nm wavelength obeys Beer's law in the range 0.020-0.090 mg L− 1 of Cu. The limit of detection calculated from a blank test (n = 10) based on 3s is 0.005 mg L− 1 of Cu. The developed procedure was applied to the analysis of water samples. The suggested DLLME is compared with two procedures previously reported from our laboratory based on (1) conventional liquid-liquid extraction, and (2) sequential injection extraction performed in a dual-valve sequential injection system. The advantages and disadvantages of each method are discussed. 相似文献
92.
Katrin Loeschner Jana Navratilova Carsten Købler Kristian Mølhave Stephan Wagner Frank von der Kammer Erik H. Larsen 《Analytical and bioanalytical chemistry》2013,405(25):8185-8195
A method of analysis of silver nanoparticles (AgNPs) in chicken meat was developed. The homogenized chicken meat sample, which was spiked with AgNPs, was subjected to enzymolysis by Proteinase K for 40 min at 37 °C. Transmission electron microscopy and inductively coupled plasma mass spectrometry (ICP-MS) in single particle mode were used to characterize the number-based size distribution of AgNPs in the meat digestate. Because similar size distributions were found in the meat digestate and in the aqueous suspension of AgNPs used for spiking the meat, it was shown that no detectable dissolution of the AgNPs took place during the sample preparation stage. The digestate was injected into the asymmetric flow field flow fractionation (AF4) -ICP-MS system, which enabled fractionation of nanoparticles from the remaining meat matrix, and resulted in one large peak in the fractograms as well as two smaller peaks eluting close to the void volume. The recovery of silver contained in the large AgNP peak was around 80 %. Size determination of AgNPs in the meat matrix, based on external size calibration of the AF4 channel, was hampered by non-ideal (early elution) behavior of the AgNPs. Single particle ICP-MS was applied for determination of the number-based particle size distribution of AgNPs in collected fractions. The presented work describes for the first time the coupling of AF4 and ICP-MS for AgNP separation in a food matrix. 相似文献
93.
rac-Bis[{(diphenylphosphino)ethyl}-phenylphosphino]methane (DPPEPM) reacts with iron(II) and ruthenium(II) halides to generate complexes with folded DPPEPM coordination. The paramagnetic, five-coordinate Fe(DPPEPM)Cl(2) (1) in CD(2)Cl(2) features a tridentate binding mode as established by (31)P{(1)H} NMR spectroscopy. Crystal structure analysis of the analogous bromo complex, Fe(DPPEPM)Br(2) (2) revealed a pseudo-octahedral, cis-α geometry at iron with DPPEPM coordinated in a tetradentate fashion. However, in CD(2)Cl(2) solution, the coordination of DPPEPM in 2 is similar to that of 1 in that one of the external phosphorus atoms is dissociated resulting in a mixture of three tridentate complexes. The chloro ruthenium complex cis-Ru(κ(4)-DPPEPM)Cl(2) (3) is obtained from rac-DPPEPM and either [RuCl(2)(COD)](2) [COD = 1,5-cyclooctadiene] or RuCl(2)(PPh(3))(4). The structure of 3 in both the solid state and in CD(2)Cl(2) solution features a folded κ(4)-DPPEPM. This binding mode was also observed in cis-[Fe(κ(4)-DPPEPM)(CH(3)CN)(2)](CF(3)SO(3))(2) (4). Addition of an excess of CO to a methanolic solution of 1 results in the replacement of one of the chloride ions by CO to yield cis-[Fe(κ(4)-DPPEPM)Cl(CO)](Cl) (5). The same reaction in CH(2)Cl(2) produces a mixture of 5 and [Fe(κ(3)-DPPEPM)Cl(2)(CO)] (6) in which one of the internal phosphines has been substituted by CO. Complexes 2, 3, 4, and 5 appear to be the first structurally characterized monometallic complexes of κ(4)-DPPEPM. 相似文献
94.
Utilization of Slovak bentonites in deposition of high-level radioactive waste and spent nuclear fuel 总被引:2,自引:0,他引:2
Michal Galambo? Ol��ga Rosskopfov�� Jana Kuf?��kov�� Pavol Rajec 《Journal of Radioanalytical and Nuclear Chemistry》2011,288(3):765-777
The basic strategic aims in the field of managing high-level radioactive waste and liquidation of nuclear power plants are all contained in the Energy policy of the Slovak Republic. Its aim is to resolve the concept of the backside of the nuclear energetics fuel cycle??long-term deposition of high-level radioactive waste and spent nuclear fuel (SNF). The most important form of high-level radioactive waste and SNF long-term deposition is their deposition in deep geological formations created by natural as well as engineering barriers used to isolate the long-lived radionuclides from the biosphere. The basic components of these barriers are clays, of which bentonite is generally referred to as the most suitable clay material. There are a few significant bentonite deposits in the Slovak Republic: Jel?ový potok, Kopernica, Lastovce, Lieskovec, Dolná Ves. The review article summarizes the information on geotechnical properties of Slovak bentonites published up-to-date, which is inevitable to know for the intention of their use. It highlights the advantages and shows drawbacks of five Slovak deposits. It suggests further research direction, to draw a thorough hydraulical, microbial and radiation profile of Slovak bentonites. 相似文献
95.
Chemical Fixation of CO2 and Other Heterogeneous Catalytic Studies by Employing a Layered Cu‐Porphyrin Prepared Through Single‐Crystal to Single‐Crystal Exchange of a Zn Analogue 下载免费PDF全文
A solvothermal reaction of Zn(NO3)2 ? 6 H2O, tetra‐(4‐pyridyl)porphyrin (H2TPyP), and 4,4′‐oxybis(benzoic acid) (H2OBA) resulted in a new two‐dimensional Zn‐ porphyrin metal–organic framework compound, [Zn2(C40H24N8)0.5(C14H8O5)(DMA)](DMA)(H2O)6 ( 1 ; DMA=N,N‐dimethylacetamide). The ZnII ions present in 1 could be exchanged by using a solution of Cu(NO3)2 ? 3 H2O in DMA at room temperature to give [Cu2(C40H24N8)0.5(C14H8O5)(DMA)](DMA)(H2O)3 ( Cu∈1 ). The extra‐framework solvent molecules have been shown to be reversibly removed or exchanged without collapse of the framework. Solvent‐free Cu∈1 was explored as an active heterogeneous catalyst towards three different organic reactions: 1) the chemical fixation of CO2 into cyclic carbonate at room temperature and 1 atm; 2) the nitroaldol reaction under solvent‐free conditions, and 3) the three‐component coupling of aminopyridine, benzaldehyde, and aryl alkynes followed by 5‐exo‐dig cyclization to produce the important pharmacophore imidazopyridine. 相似文献
96.
A novel method for the non-derivatization liquid chromatographic determination of metals (potassium, aluminium, calcium and magnesium) and organic compounds (ascorbate and aspartate) was developed and validated based on evaporative light scattering detection (ELSD). Separation of calcium, magnesium and aluminium was achieved by the cation exchange column Dionex CS-14 and an aqueous TFA mobile phase according to the following time program: 0-6 min TFA 0.96 mL L−1, 6-7 min linear gradient from TFA 0.96-6.4 mL L−1. Separation of potassium, magnesium and aspartate was achieved by the lipophilic C18 Waters Spherisorb column and isocratic aqueous 0.2 mL L−1 TFA mobile phase. Separation of sodium, magnesium, ascorbate and citrate was also achieved by the C18 analytical column, according to the following elution program: 0-2.5 min aqueous nonafluoropentanoic acid (NFPA) 0.5 mL L−1; 2.5-3.5 min linear gradient from 0.5 mL L−1 NFPA to 1.0 mL L−1 TFA. In all cases, evaporation temperature was 70 °C, pressure of the nebulizing gas (nitrogen) 3.5 bar, gain 11 and the flow rate 1.0 mL min−1. Resolution among calcium and magnesium was 1.8, while for all other separations was ≥3.2. Double logarithmic calibration curves were obtained within various ranges from 3-24 to 34-132 μg mL−1, and with good correlation (r > 0.996). Asymmetry factor ranged from 0.9 to 1.9 and limit of detection from 1.3 (magnesium) to 17 μg mL−1 (ascorbate).The developed method was applied for the assay of potassium, magnesium, calcium, aluminium, aspartate and ascorbate in pharmaceuticals and food-supplements. The accuracy of the method was evaluated using spiked samples (%recovery 95-105%, %R.S.D. < 2) and the absence of constant or proportional errors was confirmed by dilution experiments. 相似文献
97.
The first member of a new class of ditopic calix[6]arene has been synthesized, which is decorated with three N-methylimidazoles at the small rim and three 1,4-disubstituted-1,2,3-triazoles at the large rim. The coordination of a first Zn(II) cation selectively takes place at the small rim. Addition of a second equivalent results in the complexation of the three triazoles, providing a rare example of 1,2,3-triazole ligands embedded within a supramolecular system. 相似文献
98.
Secondary ion mass spectrometry and alpha-spectrometry of electrodeposited thorium films 总被引:1,自引:0,他引:1
Jozef Kuruc Jana Strišovská Dušan Galanda Silvia Dulanská Ľubomír Mátel Monika Jerigová Dušan Velič 《Journal of Radioanalytical and Nuclear Chemistry》2012,292(3):973-981
The main aim of this work was the preparation of samples with thorium content on the steel discs by electrodeposition for determination of natural thorium isotope by alpha spectrometry and secondary ion mass spectrometry and finding out their possible linear correlation between these methods. The analysis of the composition of surface was other aim of study. Discs were measured by alpha spectrometer. After that, alpha spectrometry discs were analyzed by TOF-SIMS IV, which is installed in the International Laser Centre in Bratislava. The integral and normalized intensities of isotope of 232Th and intensities of ions of ThO+, ThOH+, ThO2H+, Th2O4H+, ThO2 ?, ThO3H?, ThH3O3 ? a ThN2O5H? were measured. The linear correlation is between surface’s weights of Th and intensities of ions of Th+ from identified in SIMS spectra. We found out the chemical binding between thorium and oxygen and hydrogen on the surface of samples by SIMS method. Obtained intensities of ions 232ThO+, 232ThOH+, 232ThO2H+ prove the presence of oxidized forms of thorium in the upper layers of surface. The oxidized ions predominate in univalent form of thorium up to deep about 3,000 nm. 相似文献
99.
Marek Bučko Danica Mislovičová Jozef Nahálka Alica Vikartovská Jana Šefčovičová Jaroslav Katrlík Ján Tkáč Peter Gemeiner Igor Lacík Vladimír Štefuca Milan Polakovič Michal Rosenberg Martin Rebroš Daniela Šmogrovičová Juraj Švitel 《Chemical Papers》2012,66(11):983-998
Biological molecules such as enzymes, cells, antibodies, lectins, peptide aptamers, and cellular components in an immobilized form are extensively used in biotechnology, in biorecognition and in many medicinal applications. This review provides a comprehensive summary of the developments in new immobilization materials, techniques, and their practical applications previously developed by the authors. A detailed overview of several immobilization materials and technologies is given here, including bead cellulose, encapsulation in ionotropic gels and polyelectrolyte complexes, and various immobilization protocols applied onto surfaces. In addition, the review summarises the screening and design of an immobilization protocol, practical applications of immobilized biocatalysts in the industrial production of metabolites, monitoring, and control of fermentation processes, preparation of electrochemical/optical biosensors and biofuel cells. 相似文献
100.
Soft Phonon Modes Leading to Ultralow Thermal Conductivity and High Thermoelectric Performance in AgCuTe 下载免费PDF全文
Subhajit Roychowdhury Manoj K. Jana Jaysree Pan Satya N. Guin Prof. Dirtha Sanyal Prof. Umesh V. Waghmare Prof. Kanishka Biswas 《Angewandte Chemie (International ed. in English)》2018,57(15):4043-4047
Crystalline solids with intrinsically low lattice thermal conductivity (κL) are crucial to realizing high‐performance thermoelectric (TE) materials. Herein, we show an ultralow κL of 0.35 Wm?1 K?1 in AgCuTe, which has a remarkable TE figure‐of‐merit, zT of 1.6 at 670 K when alloyed with 10 mol % Se. First‐principles DFT calculation reveals several soft phonon modes in its room‐temperature hexagonal phase, which are also evident from low‐temperature heat‐capacity measurement. These phonon modes, dominated by Ag vibrations, soften further with temperature giving a dynamic cation disorder and driving the superionic transition. Intrinsic factors cause an ultralow κL in the room‐temperature hexagonal phase, while the dynamic disorder of Ag/Cu cations leads to reduced phonon frequencies and mean free paths in the high‐temperature rocksalt phase. Despite the cation disorder at elevated temperatures, the crystalline conduits of the rigid anion sublattice give a high power factor. 相似文献