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1.
Fumed silica nanoparticles (NanoSiO2) and chitosan (CH) based nanobiocomposite film have been used to co-immobilize rabbit-immunoglobulin antibodies (r-IgGs) and bovine serum albumin (BSA) for ochratoxin-A (OTA) detection. The observed three-dimensional (3D) arrangement of NanoSiO2 in CH matrix via hydrogen bonding, available NH2/OH groups and excellent film-forming ability of CH results in increased effective surface area of CH–NanoSiO2 nanobiocomposite for r-IgGs immobilization. Electrochemical studies suggest that presence of NanoSiO2 leads to enhanced electrochemical behaviour of CH resulting in increased electron transport between the medium and the electrode. BSA/r-IgGs/CH–NanoSiO2/ITO immunoelectrode exhibits improved sensing characteristics such as linearity (0.5–6 ng/dL), detection limit (0.3 ng/dL), response time (25 s) and sensitivity (18 μA ng/dL cm−2) with correlation coefficient as 0.98.  相似文献   

2.
The adsorption of Saccharomyces cerevisiae mandelated dehydrogenase (SCMD) protein on the surface-modified magnetic nanoparticles coated with chitosan was studied in a batch adsorption system. Functionalization of surface-modified magnetic particles was performed by the covalent binding of chitosan onto the surface of magnetic Fe3O4 nanoparticles. Characterization of these particles was carried out using FTIR spectra, transmission electron micrography (TEM), X-ray diffraction (XRD) and vibrating sample magnetometry (VSM). Magnetic measurement revealed that the magnetic Fe3O4–chitosan nanoparticles were superparamagnetic and the saturation magnetization was about 37.3 emu g−1. The adsorption capacities and rates of SCMD protein onto the magnetic Fe3O4–chitosan nanoparticles were evaluated. The adsorption capacity was influenced by pH, and it reached a maximum value around pH 8.0. The adsorption capacity increased with the increase in temperature. The adsorption isothermal data could be well interpreted by the Freundlich isotherm model. The kinetic experimental data properly correlated with the first-order kinetic model, which indicated that the reaction is the adsorption control step. The apparent adsorption activation energy was 27.62 kJ mol−1 and the first-order constant for SCMD protein was 0.01254 min−1 at 293 K.  相似文献   

3.
LiFe0.5Ti1.5O4 was synthesized by solid-state reaction carried out at 900 °C in flowing argon atmosphere, followed by rapid quenching of the reaction product to room temperature. The compound has been characterized by X-ray powder diffraction (XRD) and 57Fe Mössbauer effect spectroscopy (MES). It crystallizes in the space group P4332, a = 8.4048(1) Å. Results from Rietveld structural refinement indicated 1:3 cation ordering on the octahedral sites: Li occupies the octahedral (4b) sites, Ti occupies the octahedral (12d) sites, while the tetrahedral (8c) sites have mixed (Fe/Li) occupancy. A small, about 5%, inversion of Fe on the (4b) sites has been detected. The MES data is consistent with cation distribution and oxidation state of Fe, determined from the structural data.The title compound is thermally unstable in air atmosphere. At 800 °C it transforms to a mixture of two Fe3+ containing phases – a face centred cubic spinel Li(1+y)/2Fe(5−3y)/2TiyO4 and a Li(z−1)/2Fe(7−3z)/2TizO5 – pseudobrookite. The major product of thermal treatment at 1000 °C is a ramsdellite type lithium titanium iron(III) oxide, accompanied by traces of rutile and pseudobrookite.  相似文献   

4.
Differential scanning calorimetry and high temperature oxide melt solution calorimetry are used to study enthalpy of phase transition and enthalpies of formation of Cu2P2O7 and Cu3(P2O6OH)2. α-Cu2P2O7 is reversibly transformed to β-Cu2P2O7 at 338–363 K with an enthalpy of phase transition of 0.15 ± 0.03 kJ mol−1. Enthalpies of formation from oxides of α-Cu2P2O7 and Cu3(P2O6OH)2 are −279.0 ± 1.4 kJ mol−1 and −538.8 ± 2.7 kJ mol−1, and their standard enthalpies of formation (enthalpy of formation from elements) are −2096.1 ± 4.3 kJ mol−1 and −4302.7 ± 6.7 kJ mol−1, respectively. The presence of hydrogen in diphosphate groups changes the geometry of Cu(II) and decreases acid–base interaction between oxide components in Cu3(P2O6OH)2, thus decreasing its thermodynamic stability.  相似文献   

5.
In this paper, monodisperse Fe3O4 nanoparticles with single crystalline structure were synthesized via a facile environment-friendly method. And the size of the nanoparticles ranges from 10 nm to 15 nm. As-synthesized Fe3O4 were characterized by X-ray diffraction instrument (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FT-IR) spectrometer and field emission transmission electron microscope (FE-TEM). The effect of tartaric acid (TA) amount on products was investigated by XRD and TEM. The results indicated that TA could commendably modulate the crystalline phase, morphology and size of nanometer Fe3O4. A possible generated mechanism of Fe3O4 crystals was proposed in virtue of UV–vis absorption spectra. Besides, the magnetic properties of as-synthesized Fe3O4 were detected.  相似文献   

6.
Fe2O3/SiO2 nanocomposites based on fumed silica A-300 (SBET = 337 m2/g) with iron oxide deposits at different content were synthesized using Fe(III) acetylacetonate (Fe(acac)3) dissolved in isopropyl alcohol or carbon tetrachloride for impregnation of the nanosilica powder at different amounts of Fe(acac)3 then oxidized in air at 400–900 °C. Samples with Fe(acac)3 adsorbed onto nanosilica and samples with Fe2O3/SiO2 including 6–17 wt% of Fe2O3 were investigated using XRD, XPS, TG/DTA, TPD MS, FTIR, AFM, nitrogen adsorption, Mössbauer spectroscopy, and quantum chemistry methods. The structural characteristics and phase composition of Fe2O3 deposits depend on reaction conditions, solvent type, content of grafted iron oxide, and post-reaction treatments. The iron oxide deposits on A-300 (impregnated by the Fe(acac)3 solution in isopropanol) treated at 500–600 °C include several phases characterized by different nanoparticle size distributions; however, in the case of impregnation of A-300 by the Fe(acac)3 solution in carbon tetrachloride only α-Fe2O3 phase is formed in addition to amorphous Fe2O3. The Fe2O3/SiO2 materials remain loose (similar to the A-300 matrix) at the bulk density of 0.12–0.15 g/cm3 and SBET = 265–310 m2/g.  相似文献   

7.
Protonic ceramic membrane fuel cells (PCMFCs) based on proton-conducting electrolytes have attracted much attention because of many advantages, such as low activation energy and high energy efficiency. BaZr0.1Ce0.7Y0.2O3−δ (BZCY7) electrolyte based PCMFCs with stable Ba0.5Sr0.5Zn0.2Fe0.8O3−δ (BSZF) perovskite cathode were investigated. Using thin membrane BZCY7 electrolyte (about 15 μm in thickness) synthesized by a modified Pechini method on NiO-BZCY7 anode support, PCMFCs were assembled and tested by selecting stable BSZF perovskite cathode. An open-circuit potential of 1.015 V, a maximum power density of 486 mW cm−2, and a low polarization resistance of the electrodes of 0.08 Ω cm2 was achieved at 700 °C. The results have indicated that BZCY7 proton-conducting electrolyte with BSZF cathode is a promising material system for the next generation solid oxide fuel cells.  相似文献   

8.
The carbon coated Fe3O4 nanoparticles (Fe3O4/C) were synthesized by a simple hydrothermal reaction and applied as solid-phase extraction (SPE) sorbents to extract trace polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. The Fe3O4/C sorbents possess high adsorption capacity and extraction efficiency due to strong adsorption ability of carbon materials and large surface area of nanoparticles, and only 50 mg of sorbents are required to extract PAHs from 1000 mL water samples. The adsorption attains equilibrium rapidly and analytes are eluted with acetonitrile readily. Salinity and solution pH have no obvious effect on the recoveries of PAHs, which avoids fussy adjustment to water sample before extraction. Under optimized conditions, the detection limits of PAHs are in the range of 0.2–0.6 ng L−1. The accuracy of the method was evaluated by the recoveries of spiked samples. Good recoveries (76–110%) with low relative standard deviations from 0.8% to 9.7% are achieved. This new SPE method provides several advantages, such as high extraction efficiency, high breakthrough volumes, convenient extraction procedure, and short analysis times. To our knowledge, this is the first time that Fe3O4/C nanoparticles are used for the pretreatment of environmental water samples.  相似文献   

9.
A boronate-decorated nanomagnetic organic-inorganic hybrid material was facilely synthesized by utilizing the nanomagnetic polyhedral oligomeric silsesquioxanes (POSS) composite (Fe3O4@POSS) as the base platform. A simple copolymerization occurred between 3-acrylamidophenylboronic acid (AAPBA) and the residual end vinyl groups supplied by the substrate. Here the special emphasis was placed on the octavinyl POSS, which not only acted as the building blocks for a hybrid architecture but also facilitated the process of grafting boronate groups onto the surface of POSS based nanomagnetic composite (Fe3O4@POSS). The successful immobilization of affinity ligand-AAPBA on the Fe3O4@POSS was confirmed by Fourier transform infrared (FT-IR), elemental analysis, inductively coupled plasma atomic emission spectrometer (ICP-AES), field emission scanning electron microscope. A magnetic solid-phase extraction (MSPE) for cis-diols enrichment was developed using the as-prepared Fe3O4@POSS-AAPBA material as an affinity sorbent and three catecholamines (CAs), namely noradrenaline, epinephrine and isoprenaline, as model analytes. Under the optimal extraction conditions, sensitive and simultaneous analysis of three CAs from the urine sample was achieved by high-performance liquid chromatography with UV detection (HPLC-UV). The limits of detection (LOD, S/N = 3) and the limits of quantitation (LOQ, S/N = 10) for the target analytes were 0.81–1.32 ng mL−1 and 2.70–4.40 ng mL−1, respectively. Also good recoveries (85.5–101.7%) and repeatability (RSD≤10.1%) were obtained by this method. This work not only showed a facility for the utilization of Fe3O4@POSS as a substrate for constructing a boronate functionalized nanomagnetic sorbent, but also demonstrated the capability of the derived material for recognition of trace amount of cis-diols biomolecules presented in complicated biological matrices.  相似文献   

10.
In this report, a non-toxic method was proposed for the simple synthesis of palladium nanoparticles (Pd)/Fe3O4@C peroxidase mimetics by virtue of in situ growth of Pd nanoparticles on Fe3O4@C magnetic nanoparticles. And a microfluidic paper-based multiplex colorimetric immunodevice (named α-sheet) was developed by site-selectively immobilizing multiple antigens owing to its intrinsic high-efficiency catalytic activity of peroxidase mimetics to multiple chromogenic reactions. The immunosensor platform was prepared by growing a layer of flower-like gold nanoparticles which could entrap the primary antibodies onto paper sensing zones, and the as-prepared Pd/Fe3O4@C peroxidase mimetics was used to label secondary antibodies. In the presence of 3,3′,5,5′-tetramethylbenzidine and o-phenylenediamine chromogenic substrates, Pd/Fe3O4@C peroxidase mimetics catalyzed chromogenic reactions and showed different colors with respective intensity. To precisely identify the intensity, a piece of black wax printed chromatographic paper with three observing windows (named β-sheet) was flatted on α-sheet. Under the optimal condition, the proposed multiplex colorimetric immunodevice displayed wide linear ranges from 0.005 to 30 ng mL−1 with low detection limits of 1.7 pg mL−1 for carcinoembryonic antigen (CEA) and α-fetoprotein (α-AFP). Meanwhile, the proposed method provided provided a non-toxic, low-cost and promising tool for point-of-care diagnosis.  相似文献   

11.
Small molecules or analytes present at low concentrations are difficult to detect directly using conventional surface plasmon resonance (SPR) techniques because only small changes in the refractive index of the medium are typically induced by the binding of these analytes. Here, we present an amplification technique using core–shell Fe3O4@Au magnetic nanoparticles (MNPs) for an SPR bioassay. To evaluate this amplification effect, a novel SPR sensor based on a sandwich immunoassay was developed to detect α-fetoprotein (AFP) by immobilizing a primary AFP antibody (Ab1) on the surface of a 3-mercapto-1-propanesulfonate/chitosan-ferrocene/Au NP (MPS/CS-Fc/Au NP) film employing Fe3O4@Au–AFP secondary antibody conjugates (Fe3O4@Au–Ab2) as the amplification reagent. The stepwise fabrication of the biosensor was characterized using UV-vis spectroscopy, electrochemical impedance spectroscopy, and cyclic voltammetry. A calibration curve of Fe3O4@Au–Ab2 conjugates amplification for AFP detection was obtained to yield a correlation in the range of 1.0–200.0 ng mL−1 with a detection limit of 0.65 ng mL−1, and a significant increase in sensitivity was therefore afforded through the use of Fe3O4@Au–Ab2 conjugates as an amplifier. This magnetic separation and amplification strategy has great potential for the detection of other biomolecules of interest with low interference and high sensitivity by changing the antibody label used in the Fe3O4@Au–antibody conjugates.  相似文献   

12.
Nanocrystalline ZnMn2O4 is prepared by a polymer-pyrolysis route and used as a novel anode for lithium ion batteries. XRD and HRTEM studies reveal that the products are highly phase-pure and 30–60 nm in size. Galvanostatic cycling of ZnMn2O4 electrode at 100 mA g−1 (about 0.52 mA cm−2) between 0.01 and 3.0 V up to 50 cycles exhibits almost stable cycling performance between 10 and 50 cycles with only an average capacity fade of 0.20% per cycle and the electrode still maintains a capacity of 569 mAh g−1 after 50 cycles.  相似文献   

13.
Li2O–Cr2O3–GeO2–P2O5 based glasses were synthesized by a conventional melt-quenching method and successfully converted into glass-ceramics through heat treatment. Experimental results of DTA, XRD, ac impedance techniques and FESEM indicated that Li1.4Cr0.4Ge1.6(PO4)3 glass-ceramics treated at 900 °C for 12 h in the Li1 + xCrxGe2 − x(PO4)3 (x = 0–0.8) system exhibited the best glass stability against crystallization and the highest ambient conductivity value of 6.81 × 10−4 S/cm with an activation energy as low as 26.9 kJ/mol. In addition, the Li1.4Cr0.4Ge1.6(PO4)3 glass-ceramics displayed good chemical stability against lithium metal at room temperature. The good thermal and chemical stability, excellent conducting property, easy preparation and low cost make it promising to be used as solid-state electrolytes for all-solid-state lithium batteries.  相似文献   

14.
The Fe3O4-Prussian blue (PB) nanoparticles with core-shell structure have been in situ prepared directly on a nano-Fe3O4-modified glassy carbon electrode by cyclic voltammetry (CV). First, the magnetic nano-Fe3O4 particles were synthesized and characterized by X-ray diffraction. Then, the properties of the Fe3O4-PB nanoparticles were characterized by CV, electrochemical impedance spectroscopy, and superconducting quantum interference device. The resulting core-shell Fe3O4-PB-modified electrode displays a dramatic electrocatalytic ability toward H2O2 reduction, and the catalytic current was a linear function with the concentration of H2O2 in the range of 1 × 10−7~5 × 10−4 mol/l. A detection limit of 2 × 10−8 (s/n = 3) was determined. Moreover, it showed good reproducibility, enhanced long-term stability, and potential applications in fields of magnetite biosensors.  相似文献   

15.
The structure, conductivity and water uptake of the oxygen-deficient perovskite-type compound Ba4Ca2Ta2O11 have been investigated. Ba4Ca2Ta2O11 crystallizes in the cryolite structure (cubic, Fm3m SG) with a = 8.4508(2) Å, under dry air. The compound can be partially hydrated up to a maximum water content of approximately 0.52 mol H2O per mol Ba4Ca2Ta2O11. In moist air, the structure symmetry becomes monoclinic (C2/m) and the temperature dependence of total conductivity shows a different behavior because of changes in transport mechanism. Three regions can be observed as a function of temperature. For the low temperature range 200–400 °C, the protonic conduction is prevailing with an activation energy EA = 0.85 eV. In the intermediate temperature range (400–600 °C), O2− anionic and protonic conductions are mixed with an activation energy EA = 0.45 eV and in the third region, for temperatures above 600 °C, O2−conduction is prevailing with an activation energy EA = 0.85 eV.  相似文献   

16.
La1−x(PO3)3:Tbx3+ (0<x0.6) were prepared using solid-state reaction. The vacuum ultraviolet (VUV) excitation spectrum of La0.55(PO3)3:Tb0.453+ indicates that the absorption of (PO3)33− groups locates at about 163 and 174 nm and the absorption bands of (PO3)33− groups (174 nm) and La3+–O2− (200 nm) and Tb3+ (213 nm) overlap each other. These results imply that the (PO3)33− groups can efficiently absorb the excited energy around 172 nm and transfer the energy to Tb3+. Under 172 nm excitation, the optimal photoluminescence (PL) intensity is obtained when Tb concentration reaches 0.45 and is about 71% of commercial phosphor Zn1.96SiO4:0.04 Mn2+ with chromaticity coordinates of (0.343, 0.578) and the decay time of about 4.47 ms.  相似文献   

17.
The SrMn1−xFexO3−δ (x=1/3, 1/2, 2/3) phases have been prepared and are shown by powder X-ray and neutron (for x=1/2) diffraction to adopt an ideal cubic perovskite structure with a disordered distribution of transition-metal cations over the six-coordinate B-site. Due to synthesis in air, the phases are oxygen deficient and formally contain both Fe3+ and Fe4+. Magnetic susceptibility data show an antiferromagnetic transition at 180 and 140 K for x=1/3 and 1/2, respectively and a spin-glass transition at 5, 25, 45 K for x=1/3, 1/2 and 2/3, respectively. The magnetic properties are explained in terms of super-exchange interactions between Mn4+, Fe(4+δ)+ and Fe(3+)+. The XAS results for the Mn-sites in these compounds indicate small Mn-valence changes, however, the Mn-pre-edge spectra indicate increased localization of the Mn-eg orbitals with Fe substitution. The Mössbauer results show the distinct two-site Fe(3+)+/Fe(4+δ)+ disproportionation in the Mn- substituted materials with strong covalency effects at both sites. This disproportionation is a very concrete reflection of a localization of the Fe-d states due to the Mn-substitution.  相似文献   

18.
High-temperature proton conductors have wide applications in the areas of fuel cells, electrolysis and hydrogen separation. Barium zirconate-based materials are of interest due to their good stability and high protonic conductivity. The reported conductivity of these ceramic materials is generally less than 10−2 S/cm, even at high temperatures. This is not high enough for an electrolyte-supported device to achieve an ASR of less than 0.2 Ω cm2 therefore thin film electrolytes are required for successful application. As BaZrO3-based materials have to be sintered at temperatures as high as 1700 °C, this makes it difficult to find a suitable supporting electrode which will not undergo significant chemical reaction with the BaZrO3-based electrolyte during fabrication of the required electrode supported electrolyte. In this paper, proton-conducting BaZr0.8Y0.2O2.9 was successfully sintered at 1325 °C with a relative density of 96% via addition of 1 wt% ZnO. Fabrication of electrochemical cells using proton-conducting BaZr0.8Y0.2O2.9 as the electrolyte thus becomes possible. The formula of the 1 wt% ZnO added sample is Ba0.97Zr0.77Y0.19Zn0.04O3−δ which exhibits a tetragonal structure with space group P4/mbm (127); a=5.9787(1) Å, c=4.2345(1) Å, V=151.36(1) Å3. It was found that a solid solution was formed for a limited range of Zn doping. Conductivity has been studied as a function of atmosphere (air, dry and wet 5% H2/Ar) with the changes in bulk and grain boundary on changing atmosphere being monitored as a function of time. The total conductivity of Ba0.97Zr0.77Y0.19Zn0.04O3–δ is 1.0×10−3 S/cm above 600 °C therefore it may be used as a proton-conducting thin film electrolyte for efficient electrochemical devices at such temperatures. The grain boundary resistance is insignificant at high temperature for the well-sintered sample.  相似文献   

19.
A novel, facile and inexpensive solid phase extraction (SPE) method using ethylene glycol bis-mercaptoacetate modified 3-(trimethoxysilyl)-1-propanethiol grafted Fe3O4 nanoparticles coupled with spectrofluorimetric detection was proposed for determination of aflatoxin M1 (AFM1) in liquid milk samples. The method uses the advantage fluorescence enhancement by β-cyclodexterin complexation of AFM1 in 12% (v/v) acetonitrile–water and the remarkable properties of Fe3O4 nanoparticles namely high surface area and strong magnetization were utilized to achieve high enrichment factor (57) and satisfactory extraction recoveries (91–102%) using only 100 mg of magnetic adsorbent. Furthermore, fast separation time of about 15 min avoids many time-consuming column-passing procedures of conventional SPE. The main factors affecting extraction efficiency including pH value, desorption conditions, extraction/desorption time, sample volume, and adsorbent amount were evaluated and optimized. Under the optimal conditions, a wide linear range of 0.04–8 ng mL−1 with a low detection limit of 0.015 ng mL−1 was obtained. The developed method was applied for extraction and preconcentration of AFM1 in three commercially available milk samples and the results were compared with the official AOAC method.  相似文献   

20.
A magnetic carbon nanomaterial for Fe3O4 enclosure hydroxylated multi-walled carbon nanotubes (Fe3O4-EC-MWCNTs-OH) was prepared by the aggregating effect of Fe3O4 nanoparticle on MWCNTs-OH, and combined with high-performance liquid chromatography (HPLC)/diode array detection (DAD) to determine the aconitines (aconitine, hypaconitine and mesaconitine) in human serum samples. Compared with other extraction modes investigated in experiment, Fe3O4-EC-MWCNTs-OH sorbents showed a good affinity to target analytes. Some important parameters that could influence extraction efficiency of aconitines, including the extraction mode, amounts of Fe3O4-EC-MWCNTs-OH, pH of sample solution, extraction time, desorption solvent and desorption time, were optimized. Under optimal conditions, the recoveries of spiked serum samples were between 98.0% and 103.0%; relative standard deviations (RSDs) ranged from 0.9% to 6.2%. The correlation coefficients varied from 0.9996 to 0.9998. The limits of detection ranged from 3.1 ng mL−1 to 4.1 ng mL−1 at a signal-to-noise ratio of 3. The experimental results showed that the proposed method was feasible for the analysis of aconitines in serum samples.  相似文献   

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