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71.
纳米多孔双金属氧化物在镍钛合金纤维上的原位生长及其对多环芳烃的选择性固相微萃取 总被引:1,自引:0,他引:1
采用阳极氧化法在镍钛合金(NiTi)纤维上原位生长了双金属氧化物纳米孔(NiTiONPs)涂层,通过扫描电镜(SEM)和能谱(EDS)考察了电解质组成和电压对形貌的影响。将NiTiONPs涂层的NiTi纤维与高效液相色谱-紫外检测器联用,研究了4种典型芳香分析物的萃取性能。结果表明,富含TiO2的NiTiONPs涂层对多环芳烃(PAHs)具有良好的萃取效率,尤其对苯并[a]芘的萃取选择性优于市售聚二甲基硅氧烷纤维和聚丙烯酸酯纤维。在优化条件下,PAHs的线性范围为0.05~200μg/L,相关系数均大于0.999,检出限为0.012~0.134μg/L。对单支纤维日内和日间分析的相对标准偏差(RSDs)分别为4.0%~5.5%和6.0%~6.8%,使用分批组装的5支纤维分析的RSDs为6.4%~7.6%。实际水样分析的加标回收率为84.5%~111.5%。所制备NiTi纤维至少可重复使用250次以上,重现性好。 相似文献
72.
Makedonka D. GulcevGillian L.G. Goring Michael RakicJohn D. Brennan 《Analytica chimica acta》2002,457(1):47-59
We report on the development of reagentless fluorescence-based sensing films utilizing hydrolytic enzymes co-entrapped with polymers that are labelled with pH sensitive fluorophores. Aqueous solutions of a hydrophilic enzyme (urease) or a lipophilic enzyme (lipase) containing fluorescein or carboxy-seminaphtharhodafluor-1 (SNARF-1), either free or conjugated to a dextran polymer backbone, were mixed with hydrolyzed alkoxysilane solutions and cast onto planar surfaces to form thin, biologically active sol-gel derived films (ca. 500 nm thick). The films also contained various additives, such as methyltrimethoxysilane, dimethyldimethoxysilane, polyethylene glycol or polyvinyl alcohol, to optimize the activity of the entrapped enzymes. The photostability, leaching, pKa and pH response of the entrapped probes were characterized, as was the performance of the entrapped enzymes, and an optimal set of processing conditions was obtained for each different sensing film. In general, the results indicated that SNARF-labelled dextran was the most useful pH sensitive dye owing to insensitivity to leaching and photobleaching. Furthermore, it was observed that the pKa and pH response of this probe was insensitive to preparation conditions. The performance of the co-entrapped enzymes was highly dependent on the type and level of additive, but in all cases, it was possible to obtain active enzymes with good performance characteristics. Reagentless sensing films for urea and glyceryl tributyrate (GTB) are demonstrated based on the detection of enzyme-mediated pH changes from films coated onto planar substrates. 相似文献
73.
Wolfdieter A. Schenk 《Angewandte Chemie (International ed. in English)》1987,26(2):98-109
Donor molecules undergo dramatic changes in their chemical properties on coordination to a transition-metal atom. Highly reactive species can be trapped and studied as ligands. Conversely, stable compounds can be activated to undergo novel reactions. Sulfur dioxide complexes have generally been studied from a structural viewpoint, their reactivity having been somewhat neglected. The unstable sulfur oxides SO, S2O, and S2O2 are still often regarded as laboratory curiosities. Their successful stabilization in transition-metal complexes has now made them accessible to detailed study, in the course of which many relationships to the chemistry of SO2 complexes have become apparent. 相似文献
74.
Yingxin Liu Zuojun Wei Jiyan Zhang Wei Yan 《Reaction Kinetics and Catalysis Letters》2007,92(1):121-127
Ni-La2O3-SiO2 catalysts were prepared by wetness impregnation and sol-gel method followed by conventional drying and supercritical drying,
respectively. Their physico-chemical properties and activity for the hydrogenation of m-dinitrobenzene to m-phenylenediamine were investigated by BET, XRD, TPR, H2-TPD and activity tests. The results showed that the structural and catalytic properties of the Ni-La2O3-SiO2 catalysts obviously depended on the preparation method and the drying mode. The catalyst prepared by the sol-gel method in
combination with conventional drying exhibited the highest catalytic activity among the catalysts tested, attributable to
its well-dispersed nickel particles and larger active nickel surface area. 相似文献
75.
76.
AISI 304 Stainless Steel is widely used in different industrial fields because of its mechanical and corrosion properties.
However, its tendency to corrosion in presence of halide ions limits the applications. One strategy to improve the corrosion
resistance is the use of coatings barriers containing corrosion inhibitors in their formulation. The lanthanides present attractive
green and corrosion properties for the substitution of chromates, which are the most common substances used as corrosion protection.
However, these compounds are highly toxic, and an intense effort is being undertaken to replace them. Cerium is a good alternative
because of its relatively low cost and abundance. It fulfils the basics requirements for being considered an alternative inhibitor:
the ions form insoluble hydroxides and they present low toxicity. Inorganic and hybrid sol-gel coatings have been developed
to increase the corrosion resistance of metals and they provide an excellent vehicle for the incorporation of secondary phases
including particles and metal ions as cerium ions.
The aim of this work was to study the influence of the incorporation of cerium ions in hybrid silica sol-gel coatings deposited
on AISI 304 stainless steel as substrate as a potential replacement of chromate treatments. This system should combine the
barrier protection effect of silica coating with the corrosion inhibitor effect of the cerium ions inside the coatings. After
7 days of immersion in NaCl, coated substrates showed lower current densities than the bare steel, although the coatings produced
from Ce (III) salts experience a slight weakening in time and those obtained from Ce (IV) chemicals evidence an enhance in
the coating performance, probably due to the plugging of corrosion products in the defective areas of the film. 相似文献
77.
Jeong Hwan Kim Ji Hoon Ko Byeong-Soo Bae 《Journal of Sol-Gel Science and Technology》2007,41(3):249-255
Multi-scale hybrid nanocomposites containing both ∼15 nm silica colloids and ∼2 nm oligosiloxanes in a methacryl polymer matrix
were newly designed and fabricated. Colloidal silica sols were dispersed in methacryl oligosiloxanes nano-hybrid resins synthesized
by sol-gel reaction of methacryloxypropylmethoxysilane and diphenylsilanediol. On the basis of TEM and SANS analyses, it was
confirmed that the silica colloids were compatibly dispersed and different sizes of colloidal silica and oligosiloxanes co-exist
in the solutions. Multi-scale hybrid nanocomposites fabricated by UV and thermal curing with incorporation of silica colloids
in the nano-hybrid materials show enhanced mechanical and thermal characteristics. 相似文献
78.
A renewable three-dimensional chemically modified carbon ceramic electrode containing Ru [(tpy)(bpy)Cl] PF6 was constructed by sol-gel technique. It exhibits an excellent electro-catalytic activity for oxidation of l-cysteine and glutathione at pH range 2-8. Cyclic voltammetry was employed to characterize the electrochemical behavior of the chemically modified electrode. The electrocatalytic behavior is further exploited as a sensitive detection scheme for l-cysteine and glutathione by hydrodynamic amperometry. Optimum pH value for detection is 2 for both l-cysteine and glutathione. The catalytic rate constants for l-cysteine and glutathione were determined, which were about 2.1×103 and 2.5×103 M−1 s−1, respectively. Under the optimized condition the calibration curves are linear in the concentration range 5-685 and 5-700 μM for l-cysteine and glutathione determination, respectively. The detection limit (S/N=3) and sensitivity is 1 μM, 5 nA/μM for l-cysteine and 1 μM, 7.8 nA/μM for glutathione. The relative standard deviation (RSD) for the amperogram's currents with five injections of l-cysteine or glutathione at concentration range of linear calibration is <1.5%. The advantages of this amperometric detector are: high sensitivity, good catalytic effect, short response time (t<3 s), remarkable long-term stability, simplicity of preparation and reproducibility of surface fouling (RSD for six successive polishing is 3.31%). This sensor can be used as a chromatographic detector for analysis of l-cysteine and glutathione. 相似文献
79.
Sol-gel auto-combustion method was adopted to prepare Cd2+ ions substituted Ni–Zn nanosized ferrites having a chemical formula Ni0.5Zn0.5-xCdxFe2O4 (0.0 . Their structural, electromagnetic, and dielectric properties were investigated by using XRD, FE-SEM, EDS, FTIR, VSM, and IS. The XRD analysis revealed a single-phase cubic structure of all samples. The addition of cadmium increased the lattice constant and cell volume of Ni–Zn ferrite due to the difference in the ionic radii between Cadmium (0.97 ?Å) and Zinc (0.74 ?Å). FESEM images showed irregularly shaped grain sizes in the range of 40 to 73 ?nm with random orientations and some agglomeration. The FTIR analysis also confirmed the presence of spinal ferrite phase functional groups in all samples. The saturation magnetization decreased (from 89.51 to 71.32 emu/g) with increasing cadmium content. However, the remanent magnetization and coercivity parameters increased with an increase in cadmium content. The dc resistivity as a function of the temperature of all samples was investigated, and the activation energies were found to be in the range of 0.48 to 0.51 ?eV. The dielectric loss decreased with increasing cadmium content. However, the dielectric constant and dielectric loss tangent (tan) varied non-monotonically with increased cadmium content. 相似文献
80.
CexTi1-xO2复合氧化物的结构及负载CuO对NO还原性能研究 总被引:4,自引:1,他引:4
采用共沉淀法制备了不同摩尔比(x=0,0.1,0.2~0.9,1.0)的CexTi1-xO2复合氧化物,考察了CuO/CexTi1-xO2对NO+CO反应的活性,并用BET,TPR和XRD等技术对各试样进行了表征。结果表明,试样的结构和还原特性随焙烧温度变化而变化。XRD检测表明,x值从0.1增加到0.5时,650℃焙烧的试样已形成了CeTi2O6物相,且主要以无定形状态存在;试样经800℃焙烧后晶化完全;x>0.6时,一些TiO2已经进入了CeO2晶格,形成了Ce Ti固溶体。催化剂活性评价表明CuO/CexTi1-xO2(650℃)对NO+CO反应具有较好的活性,其活性随x值变化而变化。TPR及XRD结果表明CuO与CeTi2O6之间存在很强的相互作用,CeTi2O6物相的形成使CuO的还原峰温由380℃提前到200℃,而CuO的存在又促进CeTi2O6的还原峰温从600℃提前至200~300℃。 相似文献