Iron oxide nanoparticles within the pore system of mesoporous SBA-15 in different acidity: the synthesis and characterization

Direct hydrothermal method is employed for incorporating iron into the pore structure of SBA-15. The resultant materials were analyzed by X-ray diffraction (XRD) patterns, N₂ sorption isotherm and X-ray photoelectron spectroscopy (XPS). The characterizations of XRD patterns and XPS revealed that iron nanoparticles were present as highly dispersed nanoclusters in the well-ordered mesoporous channels of SBA-15. The characterizations of t-plot reveal only microporous channels of SBA-15 are confirmed to be filled with iron nanoparticles, leaving the mesopores unaffected. The supported material still maintained its ordered mesoporous structure similar to SBA-15 and possessed high surface area, large pore volume and uniform pore size.     

Ru/SBA-15的制备及其对水煤气变换反应的催化作用

制备了中孔分子筛SBA-15,以SBA-15为载体采用真空浸渍法制备了负载型Ru基水煤气变换反应的催化剂。利用透射电子显微镜、X-射线粉末衍射等方法对样品进行了表征。结果表明,合成的SBA-15分子筛孔径约为8 nm,粒径约为1 nm的Ru纳米粒子均匀分布在分子筛孔道中,添加适量的La2O3助剂可以显著提高催化剂的低温活性。当Ru和La2O3的负载量分别为4%和8%时,R4L8/SBA-15催化剂对CO转化率在255℃和265℃下分别达到56%和98%。     

Thermal characterisation of alumina supported chromium and platinum–chromium catalysts

This study presented results on reduction of alumina supported chromium and platinum–chromium catalysts using temperature programmed reduction method (TPR). It has been shown that catalysts after earlier oxidation step but without calcinations one undergo reduction in lower temperature in comparison to calcined only catalysts. Moreover, addition platinum to Cr/Al₂O₃ catalysts also caused decrease of reduction temperature. It has been observed that over the examined catalysts oxidation CO to CO₂ and reduction CO to CH₄ occurs. However, on Pt–Cr catalysts both reactions proceed at lower temperature compare to Cr catalysts.     

金复合介孔SBA-15吸附血红蛋白在H2O2电催化反应中的应用

以P123嵌段共聚物表面活性剂为模板剂制备介孔氧化硅SBA-15,并用沉积-沉淀(DP)法在SBA-15介孔表面负载纳米Au颗粒制备得到金复合介孔SBA-15材料(Au-SBA-15).再以Au-SBA-15材料制备玻碳修饰电极,将血红蛋白固定于修饰电极上用循环伏安法考察其对不同浓度H2O2溶液的电催化反应.在固定了血红蛋白的Hb/Au-SBA-15/GC修饰电极上,H2O2在+0.95 V处出现了氧化峰,且随着H2O2浓度的增大峰电流不断增加,说明金复合介孔氧化硅材料具有良好的生物兼容性,有利于血红蛋白的固定,其修饰电极对H2O2溶液具有一定的电催化作用.     

Synthesis and applications of mesoporous Cu-Zn-Al2O3 catalyst for dehydrogenation of 2-butanol

A series of mesoporous Cu-Zn-Al₂O₃ materials have been synthesized at ambient temperature and their structure was characterized by XRD, N₂ physical adsorption and TPR techniques. Their catalytic applications for the dehydrogenation of 2-butanol to methyl ethyl ketone (MEK) were evaluated in a fixed-bed flow reactor at atmospheric pressure. It is demonstrated from the XRD patterns that both the as-synthesized samples and calcined samples have the typical XRD patterns of meso-structured materials and the results of N₂O chemical adsorption showed that Cu was embedded in the framework of the mesoporous materials and homogeneously dispersed in the mesoporous Cu-Zn-Al₂O₃ materials. The catalytic activity of 2-butanol dehydrogenation was varied in the order of CZA(10)<CZA(CP)<CZA(20)<CZA(30); while the selectivity of MEK was increased in the order of CZA(CP)<CZA(10)<CZA(20)<CZA(30).     

On-line preconcentration and separation of Co, Ni and Cd via capillary microextraction on ordered mesoporous alumina coating and determination by inductively plasma mass spectrometry (ICP-MS)

In this paper, an ordered mesoporous alumina coating was prepared and applied to capillary microextraction (CME) of trace Co, Ni and Cd for the first time. The coated capillary was used for on-line coupling CME with inductively plasma mass spectrometry (ICP-MS) for the determination of trace metals of Co, Ni and Cd. The porous structure of Al₂O₃ coating was examined by SEM and TEM. The effects of the extraction parameters including pH, sample flow rate and volume, elution solution and interfering ions on the recovery of analytes have been investigated and optimized. Under the optimized conditions, the limits of detection were 0.33, 1.5 and 1.4 ng L⁻¹ for Co, Ni and Cd, respectively, with a preconcentration factor of 10 times. The precisions for all investigated elements were 2.7, 4.1 and 2.5% (c = 0.05 ng L⁻¹, n = 7), for Co, Ni and Cd, respectively, and the sample frequency was 8 h⁻¹.The proposed method was successfully applied for the analysis of trace metals in water, rice and urine samples with the recovery of 94-105%. In order to validate the proposed method, two certified reference materials of GBW 0913 human urine and NIES No.10-b rice flour were analyzed, and the determination values are in good agreement with the certified values. The ordered mesoporous Al₂O₃ coated capillary can be used more than 20 times without decreasing the extraction efficiency.     

Preparation and characterization of spherical mesoporous ZrO_2-Al_2O_3 composites with high thermal stability

Spherical mesoporous ZrO2-Al2O3 composites containing different zirconia content have been synthesized by an oil-column sol-gel method.A mixed alumina-zirconia hydrosol and hexamethylenetetramine solution were mixed together and added dropwise into a hot oil column.Due to the surface tension,spherical gel particles were formed in the oil column.The spherical gel particles were then aged and washed by deionized water and dried at 120 ℃ for 12 h and then calcined at 600 ℃ for 8 h,960 ℃ for 8 h or 1200 ℃ for 1...     

Chitosan–iron oxide nanobiocomposite based immunosensor for ochratoxin-A

The rabbit immunoglobulin antibodies (IgGs) have been immobilized onto nanobiocomposite film of chitosan (CH)–iron oxide (Fe₃O₄₎ nanoparticles prepared onto indium–tin oxide (ITO) electrode for detection of ochratoxin-A (OTA). Excellent film forming ability and availability of –NH₂ group in CH and affinity of surface charged Fe₃O₄ nanoparticles for oxygen support the immobilization of IgGs. Differential pulse voltammettry (DPV) studies indicate that Fe₃O₄ nanoparticles provide increased electroactive surface area for loading of IgGs and improved electron transport between IgGs and electrode. IgGs/CH–Fe₃O₄ nanobiocomposite/ITO immunoelectrode exhibits improved characteristics such as low detection limit (0.5 ng dL⁻¹), fast response time (18 s) and high sensitivity (36 μA/ng dL⁻¹ cm⁻²) with respect to IgGs/CH/ITO immunoelectrode.     

Thermal conductivity measurements on ferrofluids

The thermal conductivity of a number of ferrofluids consisting of colloidally dispersed Fe₃O₄ particles in diester, hydrocarbon, water and fluorcarbon carriers have been measured at 38°C. The variation in thermal conductivity with particle concentration is well described by Tareef's equation (1940). This has enabled the ratio of the physical to magnetic size to be determined and compared with estimates of the ratio obtained from electron micrographs and magnetic measurements.The fit between theory and experiment is particularly good for hydrocarbon carrier fluids giving the ratio of solid to magnetic radiusR _i/R _m=1.24±0.03 compared with the value obtained from magnetic data and electron micrographs of 1.19±0.07. The corresponding value from the fluids with a diester carrier ranges between 1.1<R _d/R _m<1.3 which is again consistent with microscopy and magnetic data.The application of a magnetic field of 0.1 T had no noticeable effect on the thermal conductivities of ferrofluids.     

超级铝热剂Al/Fe2O3的制备、表征及对环三亚甲基三硝胺热分解的影响

采用水热法制备了中空短棒状纳米Fe2O3,并用超声分散法将其与纳米Al颗粒复合为单金属氧化基超级铝热剂.利用X射线粉末衍射(XRD)、傅里叶变换红外(FTIR)光谱、扫描电镜及能量散射光谱仪(SEM-EDS)对样品进行表征.并运用差示扫描量热法(DSC)对比研究了超级铝热剂Al/Fe2O3、Al粉和纳米Fe2O3对环三亚甲基三硝胺(RDX)热分解特性的影响.结果表明:超级铝热剂的加入改变了RDX的热分解过程,并加剧了RDX的二次气相反应;随着超级铝热剂含量的增加,RDX的分解峰峰形发生了明显的改变;Al/Fe2O3、Al粉和Fe2O3对RDX热分解的作用主要表现为二次分解峰逐渐明显且峰温降低.     

Calixarenes functionalised water-soluble iron oxide magnetite nanoparticles for enzyme immobilisation

ABSTRACT

In this study, we first used water-soluble iron oxide nanoparticles for Candida rugosa lipase immobilisation. Moreover, two new complexation phenomena of the prepared water-soluble Fe₃O₄ nanoparticles with an enzyme might address interesting results in terms of enzyme activity and stability in typical enzymatic reactions. The catalytic activity on pH and temperature dependence, and reusability of the immobilised lipases ( p-SCX4-NP-E and p-SCX8-NP-E) were also investigated with the hydrolysis reaction of p-nitrophenyl palmitate (p-NPP). The results show that the highest catalytic affinities for p-SCX4-NP-E and p-SCX8-NP-E were obtained at pH 5.0 and pH 7.0, respectively.     

Preparation of surface plasmon resonance biosensor based on magnetic core/shell Fe3O4/SiO2 and Fe3O4/Ag/SiO2 nanoparticles

In this paper, surface plasmon resonance biosensors based on magnetic core/shell Fe(3)O(4)/SiO(2) and Fe(3)O(4)/Ag/SiO(2) nanoparticles were developed for immunoassay. With Fe(3)O(4) and Fe(3)O(4)/Ag nanoparticles being used as seeding materials, Fe(3)O(4)/SiO(2) and Fe(3)O(4)/Ag/SiO(2) nanoparticles were formed by hydrolysis of tetraethyl orthosilicate. The aldehyde group functionalized magnetic nanoparticles provide organic functionality for bioconjugation. The products were characterized by scanning electronic microscopy (SEM), transmission electronic microscopy (TEM), FTIR and UV-vis absorption spectrometry. The magnetic nanoparticles possess the unique superparamagnetism property, exceptional optical properties and good compatibilities, and could be used as immobilization matrix for goat anti-rabbit IgG. The magnetic nanoparticles can be easily immobilized on the surface of SPR biosensor chip by a magnetic pillar. The effects of Fe(3)O(4)/SiO(2) and Fe(3)O(4)/Ag/SiO(2) nanoparticles on the sensitivity of SPR biosensors were also investigated. As a result, the SPR biosensors based on Fe(3)O(4)/SiO(2) nanoparticles and Fe(3)O(4)/Ag/SiO(2) nanoparticles exhibit a response for rabbit IgG in the concentration range of 1.25-20.00 μg ml(-1) and 0.30-20.00 μg ml(-1), respectively.     

Investigation on The Thermal Properties of Fe2O(SO4)2. Part II

Fe₂O(SO₄)₂ is a secondary product of the decomposition of FeSO₄⋅H₂O. Part I of this study presents results on the synthesis of Fe₂O(SO₄)₂ in gaseous environment containing either low or high concentration of oxygen. In this paper the existence of differences between the structures of Fe₂O(SO₄)₂ and Fe₂(SO₄)₃ is proved on the basis of a detailed thermal study of Fe₂O(SO₄)₂ upon dynamic heating (differential thermal analysis) and upon isothermal heating (thermal-analytic balance) in various gaseous environments as well as by presenting kinetic data on the processes of decomposition of both compounds. This revised version was published online in July 2006 with corrections to the Cover Date.     

Adsorption and reaction studies on cobalt/alumina catalysts prepared by changing pH coprecipitation

Co/Al₂O₃ catalysts prepared by changing pH coprecipitation with Co loadings in the 8.7–36 wt.% range were analyzed by TSA, TPV, pore structure, XRD as well as CO, H₂, O₂ adsorption and CO hydrogenation. High O₂ uptake and reducibility coupled with low dispersion and constant MSA above 17 wt.% Co indicate large crystallites that are less exposed to H₂. CO hydrogenation per Co site decreases with increasing dispersion or decreasing metal loading.     

Controlled assembly of superparamagnetic iron oxide nanoparticles on electrospun PU nanofibrous membrane: A novel heat-generating substrate for magnetic hyperthermia application

A facile method of fabricating novel heat-generating membranes composed of electrospun polyurethane (PU) nanofibers decorated with superparamagnetic iron oxide nanoparticles (NPs) is reported. Electrospinning was used to produce polymeric nanofibrous matrix, whereas polyol immersion technique allowed in situ assembly of well-dispersed Fe₃O₄ NPs on the nanofibrous membranes without any surfactant, and without sensitizing and stabilizing reagent. The assembly phenomena can be explained by the hydrogen-bonding interactions between the amide groups in the PU matrix and the hydroxyl groups capped on the surface of the Fe₃O₄ NPs. The prepared nanocomposite fibers showed acceptable magnetization value of 33.12 emu/g, after measuring the magnetic hysteresis loops using SQUID. Moreover, the inductive heating property of electrospun magnetic nanofibrous membranes under an alternating current (AC) magnetic field was investigated. We observed a progressive increase in the heating rate with the increase in the amount of magnetic Fe₃O₄ NPs in/on the membranes. The present electrospun magnetic nanofibrous membrane may be a potential candidate as a novel heat-generating substrate for localized hyperthermia cancer therapy.     

The Thermal Properties and Firing Characteristics of Zr/KClO4 Priming Compositions Containing Graphite,Fe2O3 and Al2O3 additives

Thermal decomposition of Zr/KClO₄ priming compositions containing different concentration of additives, such as graphite, Fe₂O₃ and Al₂O₃ have been studied by DSC/TG techniques. The firing characteristics of these primer mixtures have also been examined by Bruceton test and by adiabatic calorimeter. The results of these experiments suggest that strong interaction has been occurred between KClO₄ and Fe₂O₃ in the solid state. This revised version was published online in July 2006 with corrections to the Cover Date.     

Magnetic assembled electrochemical platform using Fe2O3 filled carbon nanotubes and enzyme

A novel electrochemical nanostructured biosensor based on carbon nanotubes (CNTs) has been constructed by magnetic assembly method. The magnetic multi-walled carbon nanotubes (M-MWNTs) were prepared by introducing Fe₂O₃ nanoparticles into the nanotubes. Thus the multilayered functional platform could be assembled with the aid of magnetic field. The horseradish peroxidase (HRP) was employed as a model enzyme to demonstrate the final performance of the nanostructured biosensor. SEM, UV–vis spectroscopy and electrochemical techniques were used for characterization of assembly process. The resulting three-dimensional M-MWNTs/HRP multilayer films have showed satisfactory stability, biocompatibility and electrochemical properties.     

Selective catalytic oxidation of NO over iron and manganese oxides supported on mesoporous silica

The selective catalytic oxidation （SCO） of NO was studied on a catalyst consisting of iron-manganese oxide supported on mesoporous silica （MPS） with different Mn/Fe ratios. Effects of the amount of manganese and iron, oxygen, and calcination temperature on NO conversion were also investigated. It was found that the Mn-Fe/MPS catalyst with a Mn/Fe molar ratio of 1 showed the highest activity at the calcination temperature of 400 °C. The results showed that over this catalyst, NO conversion reached 70% under the condition of 280 °C and a space velocity of 5000 h-1. SO2 and H2O had no adverse impact on the reaction activity when the SCO reaction temperature was above 240 °C. In addition, the SCO activity was suppressed gradually in the presence of SO2 and H2O below 240 °C, and such an effect was reversible after heating treatment.     

钛铁矿制备二氧化钛-四氧化三铁复合材料及其光催化应用

TiO_2因具有多种优异的特性被广泛应用在半导体光催化领域,但是纳米结构的TiO_2颗粒细微,在进行光催化反应之后,难以回收再利用。本文以廉价钛铁矿为原料制备光催化剂TiO_2,同时利用副产物铁合成Fe_3O_4,并采用简单温和的浸渍法制备Fe_3O_4/TiO_2磁性复合材料。通过XRD、FT-IR、SEM、EDS等手段对材料形态结构进行表征分析,并以光降解有机污染物若丹明B为探针反应,考察其光催化性能。结果表明,质量比为1∶10的Fe_3O_4/TiO_2复合材料结构稳定、分散均匀,具有最优的光催化活性(波长356nm下反应3h,若丹明B降解率达到64.0%),并表现出良好的重复性。同时,动力学结果显示降解符合一级反应动力学。     

Determination of Hydrogen Peroxide Using a Novel Sensor Based on Fe3O4 Magnetic Nanoparticles

Fe₃O₄ magnetic nanoparticles were synthesized by chemical co-precipitation with sodium citrate as a surfactant and were used with chitosan to construct a novel hydrogen peroxide sensor. The electrochemical behavior of hydrogen peroxide at the sensor was investigated by cyclic voltammetry. The composite film electrocatalyzed the reduction of hydrogen peroxide, and the peak current increased linearly with concentration from 1.00 × 10^?5 to 1.00 × 10^?3 mol · L^?1 (R = 0.9974) with a detection limit of 1.53 × 10^?6 mol · L^?1. This novel nonenzyme sensor provided good sensitivity, stability, and precision with potential applications.