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1.
natCd electrodeposition on a copper substrate was investigated for production of 111In radionuclide. The electrodeposition experiments were carried out by alkaline plating baths. Operating parameters such as pH, temperature, and current density are also optimized. The current efficiency was measured at different current densities. The optimum conditions of the cadmium electrodeposition were as follows: 2.35 g L−1 cadmium, pH = 13, DC current density of ca 4.27 mA cm−2 at 25 °C temperature with 62.48 μm thickness. SEM photomicrographs demonstrated fine-grained structure of the deposit obtained from the optimum bath.  相似文献   

2.
This article presents, 122Sb (T 1/2 = 2.723 days, I β- = 97.59%) was produced via the natSn(p,xn) nuclear process at the AMIRS (Cyclone-30, IBA, Belgium). The electrodeposition experiments were carried out by potassium stannate trihydrate (K2Sn(OH)6) and potassium hydroxide. The optimum conditions of the electrodeposition of tin were as follows: 40 g/L natSn, 20 g/L KOH, 115 g/L K2Sn(OH)6, DC current density of 5 A/dm2 with a bath temperature of 75 °C. The electroplated Tin-target was irradiated with 26.5 MeV protons at current of 180 μA for 20 min. Solvent extraction of no-carrier-added 122Sb from irradiated Tin-natural target hydrochloric solution was investigated using di-n-butyl ether (C8H18O). Yields of about 3.61 MBq/μAh were experimentally obtained.  相似文献   

3.
The electroplating of zinc is carried out in an alkaline cyanide bath. Operating parameters such as pH, temperature, and current density and amount of the electrolyte components are optimized. The optimum conditions of the electrodeposition of zinc were as follows: 2.7 g L−1 ZnO, 7.1 g L−1 KCN, 11.1 g L−1 KOH, pH = 13–14, DC current density of ca 8.55 mA cm−2 at 40–50 °C temperature with 89% current efficiency. SEM photomicrographs revealed fine-grained structure of the deposit from the bath.  相似文献   

4.
Treatment of FeCl3 with 1 equiv of 3-(pyrid-2-yl)-5-(tertbutyl)-1H-pyrazole (L) in basic methanol affords crystalline [Fe3Cl5(μ 3-O)(μ-OMe)2L2(MeOH)] in moderate yield. The compound has an unusual isosceles triangular [Fe3(μ 3-O)(μ-OMe)2]5+ core with one unbridged edge. Two of the iron(III) centres in the compound are approximately octahedral, while the third has a five-coordinate geometry. Magnetic susceptibility measurements show antiferromagnetic coupling between the iron centres, leading to a S = 3/2 magnetic ground state and S = 5/2 excited state that are almost accidentally degenerate according to simulation. An analogous reaction using Fe[ClO4]3 as starting material instead affords the low-spin iron(II) complex [FeL3][ClO4]2.  相似文献   

5.
(BiFeO3)1−x –(BaTiO3) x solid solution thin films are grown on Pt/Ti/SiO2/Si substrates by chemical solution deposition method. Films with x = 0.00, 0.05 and 0.10 were prepared by annealing at 500°C. X-ray diffraction patterns indicate that the pure BiFeO3 film adopts random orientation while the solid solution films are highly (100) preferentially oriented. Improved electric property at room temperature was observed in the BaTiO3 incorporated BiFeO3 films. The remanent polarization of the film with x = 0.0, 0.05 and 0.10 are 76.6, 51.9 and 19.7 μC/cm2 respectively under a measuring electric field of 0.94 MV/cm. The BaTiO3 incorporated BiFeO3 films show improved fatigue endurance. By the solid solution with BaTiO3, the leakage current density is reduced effectively.  相似文献   

6.
The present work reports on the synthesis, characterization and performance of a new iron(III)-containing ionic liquid [(C4H9)2-bim][FeCl4] (Fe-IL, bim = benzimidazolium) as an electrocatalyst for nitrite and bromate reduction. The melting point of Fe-IL is 70 °C. Thermal behavior of the Fe-IL was studied by differential scanning calorimetry and thermalgravimetry. The value of magnetic moment and its temperature dependence were measured. A conductive carbon paste electrode (Fe-IL/CPE) comprised of Fe-IL and carbon powder was fabricated by the direct mixing method. The Fe-IL has double functions—a binder and an electrocatalyst. The electrochemical behavior and electrocatalysis of Fe-IL/CPE have been studied by cyclic voltammetry. The Fe-IL/CPE shows excellent electrocatalytic activities toward nitrite and bromate reduction. The detection limit and the sensitivity are 0.01 μM and 100.58 μA μM−1 for nitrite, and 0.01 μM and 83.11 μA μM−1 for bromate detection, respectively. This work demonstrates that the Fe-IL may become a new kind of functional material in constructing chemicals and biosensors.  相似文献   

7.
A magnetic mesoporous carbon material (i.e., mesoporous iron oxide/C, mesoFe/C) is synthesized for protein immobilization, using glucose oxidase (GOx) as model. Transmission electron microscopy images show that mesoFe/C has highly ordered porous structure with uniform pore size, and iron oxide nanoparticles are dispersed along the wall of carbon. After adsorption of GOx, the GOx-mesoFe/C composite is separated with magnet. The immobilized GOx remains its natural structure according to the reflection–absorption infrared spectra. When the GOx-mesoFe/C composite is coated on a Pt electrode surface, the GOx gives a couple of quasireversible voltammetric peaks at −0.5 V (vs. saturated calomel electrode) due to the redox of FAD/FADH2. The electron-transfer rate constant (k s) is ca. 0.49 s−1. The modified electrode presents remarkably amperometric response to glucose at 0.6 V. The response time (t 95%) is less than 6 s; the response current is linear to glucose concentration in the range of 0.2–10 mM with a sensitivity of 27 μA mM−1 cm−2. The detection limit is 0.08 mM (S/N = 3). The apparent Michaelis–Menten constant (K mapp) of the enzyme reaction is ca. 6.6 mM, indicating that the GOx immobilized with mesoFe/C has high affinity to the substrate.  相似文献   

8.
Mannich reaction of 2-Amino propanol, 2-tert-butyl-4-methylphenol, and formaldehyde in the ratio of 1:2:2 provides a new compound, N-(1-propanol)-N,N-bis(3-tert-butyl-5-methyl-2-hydroxybenxyl)amine (H3L), which has been characterized by X-ray crystallography and elemental analysis. In the presence of Et3N, the reaction of H3L and FeCl3·6H2O gives a dinuclear Fe(III) complex [Fe2L2] 1, which has been characterized by X-ray crystallography, magnetic measurement, and cyclic voltammetry. The value of μeff at room temperature (5.97 μB) is much less than the expected spin-only value (8.37 μB) of two high spin (hs) Fe3+ (S = 5/2) ions [μ = g[∑ZS(S + 1)]1/2], indicating there are strong coupling interactions between Fe3+ ions. The magnetic behavior of 1 denotes the occurrence of intramolecular antiferromagnetic interactions (J = −13.35 cm−1 ). CV of 1 reveals two reversible waves at 0.433 and 1.227 V versus AgCl/Ag, which can be ascribed to the successive redox coupling of FeIIFeII/FeIIIFeII and FeIIIFeII/FeIIIFeIII, respectively.  相似文献   

9.
Pyrroloquinoline quinone (PQQ), an essential nutrient, antioxidant, redox modulator and nerve growth factor found in a class of enzymes called quinoproteins, was labeled with 99mTc by using stannous fluoride (SnF2) method. Radiolabeling qualification, quality control and characterization of 99mTc-PQQ and its biodistribution studies in mice were performed and discussed. Effects of pH values, temperature, time and reducing agents concentration on the radiolabeling yield were investigated. The quality control procedure of 99mTc-PQQ was determined by thin layer chromatography (TLC), radio high-performance liquid chromatography (RHPLC) and paper electrophoresis methods. The average radiolabeling yield was 94 ± 1% under optimum conditions of 0.99 mg of PQQ, 30 μg of SnF2, 0.5 mg of ethylenediaminetetraacetic acid disodium salt (EDTA-2Na) and 18.5 MBq of Na99mTcO4 at pH 6 and 25 °C with a response volume of 1 ± 0.1 mL. 99mTc-PQQ was stable and anionic. Lipid–water partition coefficient of 99mTc-PQQ was −1.49 ± 0.16. The pharmacokinetics parameters of 99mTc-PQQ were t 1/2α = 18.16 min, t 1/2β = 100.45 min, K 12 = 0.013 min−1, K 21 = 0.017 min−1, K e = 0.016 min−1, AUC (area under the curve) = 1040.78 ID% g−1 min and CL (plasma clearance) = 0.096 mL min−1. The dual-exponential equation was Y = 10.88e−0.038t  + 5.21e−0.0069t . The biodistribution of 99mTc-PQQ was studied in ICR (Institute for Cancer Research 7701 Burhelme Are., Fox Chase, Philadelphia, PA 1911 USA) mice. In vitro autoradiographic studies clearly showed that the 99mTc-PQQ radioactivity accumulated predominantly in the hippocampus and cortex, which had a high density of N-methyl-d-aspartate Receptor (NMDAR). The enrichment can be blocked by NMDAR redox modulatory site antagonists-ebselen (EB) and 99mTc-PQQ is therefore a promising candidate for the molecular imaging of NMDAR. To date, however, there have been no studies characterizing 99mTc-PQQ.  相似文献   

10.
The electrodeposition of ternary zinc–nickel–iron alloy was studied in acidic sulfate bath. The comparison between Zn, Ni, and Fe deposition and Zn–Ni and Zn–Ni–Fe co-deposition revealed that the remarkable inhibition of Ni and Fe deposition takes place due to the presence of Zn2+ in the plating bath. The increase in corrosion resistance of ternary deposits is not only attributed to the formation of γ-Ni2Zn11 phase but also to iron co-deposition and formation of iron phase. It was also found that the bath temperature has a great effect on the surface appearance and the deposit composition. The investigation was carried out using cyclic voltammetry and galvanostatic techniques for electrodeposition, while linear polarization resistance and anodic linear sweeping voltammetry techniques were used for corrosion study. Morphology and chemical composition of the deposits were characterized by means of scanning electron microscopy and atomic absorption spectroscopy.  相似文献   

11.
Bi1−x Ce x FeO3 (x = 0, 0.05, 0.1, 0.15 and 0.20) (BCFO) thin films were deposited on Pt/TiN/Si3N4/Si substrates by sol–gel technique. Crystal structures, surface chemical compositions and bonding states of BCFO films were investigated by X-ray diffraction and X-ray photoelectron spectroscopy (XPS), respectively. Compared to BiFeO3 (BFO) counterparts, the fitted XPS narrow-scan spectra of Bi 4f7/2, Bi 4f5/2, Fe 2p3/2, Fe 2p1/2 and O 1s peaks for Bi0.8Ce0.2FeO3 film shift towards higher binding energy regions by amounts of 0.33, 0.29, 0.43, 0.58 and 0.49 eV, respectively. Dielectric constants and loss tangents of the BCFO (x = 0, 0.1 and 0.2) film capacitors are 159, 131, 116, 0.048, 0.041 and 0.035 at 1 MHz, respectively. Bi0.8Ce0.2FeO3 film has a higher remnant polarization (P r = 2.04 μC/cm2) than that of the BFO (P r = 1.08 μC/cm2) at 388 kV/cm. Leakage current density of the Bi0.8Ce0.2FeO3 capacitor is 1.47 × 10−4 A/cm2 at 388 kV/cm, which is about two orders of magnitude lower than that of the BFO counterpart. Furthermore, Ce cations are feasibly substituted for Bi3+ in the Bi0.8Ce0.2FeO3 matrix, possibly resulting in the enhanced ferroelectric properties for the decreased grain sizes and the reduced oxygen vacancies.  相似文献   

12.
Phenylalanine dehydrogenase (l-PheDH) from Sporosarcina ureae was immobilized on DEAE-cellulose, modified initially with 2-amino-4,6-dichloro-s-triazine followed by hexamethylenediamine and glutaraldehyde. The highest activity of immobilized PheDH was determined as 95.75 U/g support with 56% retained activity. The optimum pH value of immobilized l-PheDH was shifted from pH 10.4 to 11.0. The immobilized l-PheDH showed activity variations close to the maximum value in a wider temperature range of 45–55 °C, whereas it was 40 °C for the native enzyme. The pH and the thermal stability of the immobilized l-PheDH were also better than the native enzyme. At pH 10.4 and 25 °C, K m values of the native and the immobilized l-PheDH were determined as K m Phe = 0.118, 0.063 mM and K m NAD+ = 0.234, 0.128 mM, respectively. Formed NADH at the exit of packed bed reactor column was detected by the flow-injection analysis system. The conversion efficiency of the reactor was found to be 100% in the range of 5–600 μM Phe at 9 mM NAD+ with a total flow rate of 0.1 mL/min. The reactor was used for the analyses of 30 samples each for 3 h per day. The half-life period of the reactor was 15 days.  相似文献   

13.
The difurylphosphido-bridged dinuclear complex [Ru2(CO)6(μ-PFu2)(μ-η12-Fu)] (Fu = 2-furyl) 1 readily reacts with two equivalents of each of the terminal alkynes HC≡CR (R = Fc, p-C6H4Fc, p-C6H4NO2, Fc = Fe(η5-C5H5)(η5-C5H4)) by an interesting head-to-tail ynyl coupling with a furan group to form a series of phosphido-bridged diruthenium compounds containing a novel furyl-substituted C4 hydrocarbyl chain of stoichiometry [Ru2(CO)4(μ-PFu2){μ-η1123-RCC(H)C(R)C(H)Fu}] (R = Fc 2, p-C6H4Fc 3, p-C6H4NO2 4) in moderate to good yields. Reaction of 1 with an equimolar amount of HC≡CFc and HC≡C(p-C6H4NO2) afforded a pair of isomers of [Ru2(CO)4(μ-PFu2){μ-η1123-R1CC(H)C(R2)C(H)Fu}] (R1 = Fc, R2 = p-C6H4NO2 5a; R1 = p-C6H4NO2, R2 = Fc 5b) together with a small mixture of 4. X-ray crystal structures of 2, 3, 5a and 5b are reported. All of these new alkyne-derived dinuclear complexes are electron precise with 34 cluster valence electrons in which the μ-η12-furyl ligand acts as a three-electron donor and the μ-phosphido Ru2 framework is retained in the products upon alkyne coupling reactions. The resulting organic fragment of each complex is coordinated to the Ru atoms via a π, a π-allyl and two σ bonds, and donates seven electrons to the metal core. Dedicated to the memory of Professor F. Albert Cotton.  相似文献   

14.
A heterobimetallic cyano-bridged 1D coordination polymer of the composition [Ni(baepn)(μ-NC)Fe(CN)3(NO)(μ-CN)]n·3H2O has been synthesized by the reaction of nickel(II) nitrate hexahydrate, baepn (baepn = N, N′-bis(2-aminoethyl)-1,3-propanediamine), and sodium nitroprusside dihydrate in a methanol–water mixture. The complex was characterized by physicochemical and spectroscopic methods. The crystal structure was established by single-crystal X-ray diffraction analysis. It reveals cyano-bridged heterometallic chains consisting of alternating arrays of Ni(II) and Fe(II) atoms, both being embedded in distorted octahedral environments. Low-temperature susceptibility measurements show the presence of weak antiferromagnetic exchange interactions between paramagnetic Ni(II) centers (J = −0.46 cm−1) through long diamagnetic [Fe(CN)5(NO)]2− bridges. Spin state of the iron atom was established by 57Fe M?ssbauer spectroscopy.  相似文献   

15.
Highly (100)-oriented Pb0.8La0.1Ca0.1Ti0.975O3 (PLCT) thin films deposited on Pt/Ti/SiO2/Si substrate were successfully achieved by a sol–gel route. The influence of annealing temperature on microstructures and electric properties was investigated; it was found that the PLCT film could be crystallized only at 450 °C. When the annealing temperature increased to 500 °C, the PLCT film exhibited highly (100)-oriented, which also possessed higher remnant polarization Pr (27 μC/cm2) and better pyroelectric figure of merit (F d = 205 μC/m2k) at room temperature. It was also found too high annealing temperature (625 °C) could lead to recrystallization of film, and the small grains caused by recrystallization could make polarization reversal difficult and disturbed the preferred crystal growth in film, which was not benefit to obtain enhanced electric properties.  相似文献   

16.
The electrochemical solid phase micro-extraction of salicylic acid (SA) at graphite-epoxy-composed solid electrode surface was studied by cyclic voltammetry. SA was oxidized electrochemically in pH 12.0 aqueous solution at 0.70 V (vs. saturated calomel electrode) for 7 s. The oxidized product shows two surface-controlled reversible redox couples with two proton transferred in the pH range of 1.0∼6.0 and one proton transferred in the pH range of 10.0∼13.0 and is extracted on the electrode surface with a kinetic Boltzman function of i p = 3.473–4.499/[1 + e(t − 7.332)/6.123] (χ 2 = 0.00285 μA). The anodic peak current of the extracted specie in differential pulse voltammograms is proportional to the concentration of SA with regression equation of i p = −5.913 + 0.4843 c (R = 0.995, SD = 1.6 μA) in the range of 5.00∼200 μM. The detection limit is 5.00 μM with RSD of 1.59% at 60 μM. The method is sensitive and convenient and was applied to the detection of SA in mouse blood samples with satisfactory results.  相似文献   

17.
The Rh target preparation for production of 103Pd was investigated by using a thick electrodeposition of rhodium metal on a copper backing. The electrodeposition experiments were performed in acidic sulfate media using RhCl3·3H2O, Rh2(SO4)3 (recovered from hydrochloric acid solution) and also in the commercially available Rhodex plating baths. For high current beam irradiation of a Rh target, the qualities of the deposit of the three baths were compared in terms of thermal shock, crack-free and morphology criteria. The quality of the plating obtained from a sulfate bath [Rh2(SO4)3] was comparable with the one obtained from commercially available Rhodex bath. The optimum conditions of the electrodepositions were as follows: 4.8 g rhodium [as Rh2(SO4)3], pH 2, DC current density of ca 8.5 mA·cm–2, 1% sulfamic acid (w/v) and temperature 40–60 °C.The authors would like to thank their colleagues at the VUB-Cyclotron department for help and assistance in preparation of the electrodeposition equipment and taking the SEM photomicrographs and also K. Aardaneh (NRCAM) for his assistance.  相似文献   

18.

Abstract  

A series of 1-D lanthanide coordination polymers [Ln(μ3-OH)(pybz)(pa)] n (Ln = Er (1), Tb (2), Gd (3), Hpybz = 4-pyridin-4-yl-benzoic acid, Hpa = 2-picolinic acid) based on [Ln43-OH)4] cluster units have been hydrothermally synthesized and characterized by single crystal X-ray diffraction, IR, elemental analysis, and thermogravimetric analysis. X-ray crystal structure analyses reveal that 1–3 are isomorphous with tetragonal space group P [`4] \overline{4} 21c and comprise tetranuclear Ln–O clusters, in which four Ln3+ centers are joined together by four μ3-bridging hydroxyl groups to form cubane-like [Ln43-OH)4]8+ cores that are further linked by four μ3-pa ligands to produce 1-D chains along the c-axis.  相似文献   

19.
Abstract  Monoclinic crystals of [Cu2(μ-I)2(PPh3)2(μ-N, S-pymSH)] · CH3CN) (1), were obtained by equimolar reaction of copper(I) iodide with pyrimidine-2-thione (pymSH), followed by the addition of triphenylphosphine (PPh3) in acetonitrile. Crystal data for 1: space group P21, Z = 2, a = 9.896, b = 18.378, c = 11.703 ?, β = 101.73°. It has an iodo-bridged Cu(μ-I)2Cu core and the pyrimdine-2-thione binds to both Cu centers via N, S-bridging across the Cu(μ-I)2Cu core. This N, S-bridging, a rare coordination mode for pyrimidine-2-thione, leads to a short Cu···Cu separation of 2.675(2) ? (sum of van der Waals radius of Cu atoms, 2.80 ?). The geometry around each Cu center is distorted tetrahedral with angles varying in the range, ca. 102–119°. Copper(I) chloride and bromide also yielded monoclinic crystals of S-bonded tetrahedral monomers, [CuBr(pymSH)(PPh3)2] 2 and [CuCl(pymSH)(PPh3)2] 3. Crystal data for 2: space group P21/n, Z = 8, a = 12.825, b = 43.122, c = 13.396 ?, β = 90.79°. Crystal data for 3: space group P21/c, Z = 4, a = 14.340, b = 10.111, c = 24.200 ?, β = 94.36°. Compound 2 has two crystallographically independent molecules in crystal lattice. The 31P NMR spectrum of 1 showed two signals for PPh3 ligands bonded to two Cu centers with different coordination cores: CuI2PN and CuI2PS. Both 2 and 3 showed one signal each for PPh3 in their 31P NMR spectra. Graphical abstract  Reaction of copper(I) iodide with pyrimidine-2-thione and triphenylphosphine formed monoclinic crystals of dimer 1 with unusual N, S-bridging across Cu(μ2-I)2Cu core.   相似文献   

20.
The Rh target preparation for production of 103Pd was investigated by using a thick electrodeposition of rhodium metal on a copper backing. The electrodeposition experiments were performed in acidic sulfate media using RhCl3·3H2O, Rh2(SO4)3 (recovered from hydrochloric acid solution) and also in the commercially available Rhodex plating baths. For high current beam irradiation of a Rh target, the qualities of the deposit of the three baths were compared in terms of thermal shock, crack-free and morphology criteria. The quality of the plating obtained from a sulfate bath [Rh2(SO4)3] was comparable with the one obtained from commercially available Rhodex bath. The optimum conditions of the electrodepositions were as follows: 4.8 g rhodium [as Rh2(SO4)3], pH 2, DC current density of ca 8.5 mA·cm–2, 1% sulfamic acid (w/v) and temperature 40–60 °C.The authors would like to thank their colleagues at the VUB-Cyclotron department for help and assistance in preparation of the electrodeposition equipment and taking the SEM photomicrographs and also K. Aardaneh (NRCAM) for his assistance.  相似文献   

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