Preparation of nanosized titania by hydrolysis of alkoxide titanium in micelles

Nanosized titania particles, with typical particle sizes in the range of 30-50 nm have been synthesized using a microemulsion-mediated process. In this process, the aqueous cores of microemulsions have been used as constrained microreactors for the precipitation of titania precursor. The microemulsion was provided by a functionalized surfactant derived from the commercially available mixtures of sorbitol monooleate and polysorbate 80 (abbreviated as Span-Tween 80). The hydroxide particles, produced by the hydrolysis of the titanium tetraisopropoxide in the water droplets containing surfactant, were separated, dried, and calcined to form nanoparticles of TiO₂. The dependence of the size of the precipitated TiO₂ particles on various structure parameters of the microemulsion was studied in detail.     

Synthesis of nanocrystalline titanium nitride by reacting titanium dioxide with sodium amide

A new method for synthesis of nanocrystalline titanium nitride was developed through the reaction of titanium oxide and sodium amide at 500–600 °C for 12 h in an autoclave. X-ray diffraction (XRD) and electron diffraction (SAED) results indicated the product had a cubic phase with lattice parameter a = 4.242 Å. Transmission electron microscopy (TEM) and field emission scanning electron microscopy (FESEM) revealed that the particle sizes were 10 to 40 nm. Quantitative analysis using X-ray photoelectron spectrum (XPS) showed the atomic ratio Ti:N was 1.03:1.     

Photocatalytic degradation of dyes and organic contaminants in water using nanocrystalline anatase and rutile TiO2

Nanocrystalline TiO₂ was synthesized by controlled hydrolysis of titanium tetraisopropoxide. The anatase phase was converted to rutile phase by thermal treatment at 1023 K for 11 h. The catalysts were characterized by X-ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), Fourier-transform infrared absorption spectrophotometry (FT-IR) and N₂ adsorption (BET) at 77 K. This study compare the photocatalytic activity of the anatase and rutile phases of nanocrystalline TiO₂ for the degradation of acetophenone, nitrobenzene, methylene blue and malachite green present in aqueous solutions. The initial rate of degradation was calculated to compare the photocatalytic activity of anatase and rutile nanocrystalline TiO₂ for the degradation of different substances under ultraviolet light irradiation. The higher photocatalytic activity was obtained in anatase phase TiO₂ for the degradation of all substances as compared with rutile phase. It is concluded that the higher photocatalytic activity in anatase TiO₂ is due to parameters like band-gap, number of hydroxyl groups, surface area and porosity of the catalyst.     

Photocatalytic degradation of dyes and organic contaminants in water using nanocrystalline anatase and rutile TiO2

Nanocrystalline TiO₂ was synthesized by controlled hydrolysis of titanium tetraisopropoxide. The anatase phase was converted to rutile phase by thermal treatment at 1023 K for 11 h. The catalysts were characterized by X-ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), Fourier-transform infrared absorption spectrophotometry (FT-IR) and N₂ adsorption (BET) at 77 K. This study compare the photocatalytic activity of the anatase and rutile phases of nanocrystalline TiO₂ for the degradation of acetophenone, nitrobenzene, methylene blue and malachite green present in aqueous solutions. The initial rate of degradation was calculated to compare the photocatalytic activity of anatase and rutile nanocrystalline TiO₂ for the degradation of different substances under ultraviolet light irradiation. The higher photocatalytic activity was obtained in anatase phase TiO₂ for the degradation of all substances as compared with rutile phase. It is concluded that the higher photocatalytic activity in anatase TiO₂ is due to parameters like band-gap, number of hydroxyl groups, surface area and porosity of the catalyst.     

Synthesis of soluble and thermally stable polyimides with phthalimide as pendent group from pyridine-containing triamine

We report the design and synthesis of a novel pyridine-containing triamine monomer, 2,6-bis(4-aminophenyl)-4-(4-aminophenoxy)pyridine (BAAP), through combining the nucleophilic aromatic substitution with modified Chichibabin reaction and hydrazine hydrate reduction. Based on it, a novel three-step route was applied in order to obtain a series of new polyimides, containing phthalimide as pendent group and pyridine moieties in main chains. The three-step route consisted of terminating the triamine by incorporating phthalic amic acid as pendant, ring-opening polymerization to form poly(amic acid)s and further chemical imidization to acquire polyimides. Nuclear Magnetic Resonance Spectroscopy (¹H-NMR) was used for chemical structural characterization, and the results indicated the various forms of BAAP and branched structure units in the obtained polyimides. The morphology structures of the polyimides were evaluated by X-ray diffraction patterns, and the d-spacing values were found in the range of 4.14–4.65 ?. Most of the resulting polyimides were soluble in polar aprotic solvents, such as NMP, DMF, DMAc, DMSO, and so on. Meanwhile, the polyimides exhibited excellent thermal stability, with the decomposition temperature at 5 and 10 % weight loss temperatures in the ranges of 399.1–461.1 °C and 481.1–566.9 °C, respectively. The polyimides, based on 6FDA, possessed the best comprehensive thermally stable and soluble performance.     

自动固相萃取与气相色谱--质谱联用测定水中有机磷农药

采用自动固相萃取法预处理,用气相色谱-质谱仪测定有机磷农药。最低检出限在0.10~0.30mg/L之间,水样加标回收率为75%~105%,样品经5次重复测定后相对标准偏差均小于6.0%。结果表明,该法具有简单、快速、准确的特点。     

Identification of organic acids in secondary organic aerosol and the corresponding gas phase from chamber experiments

Organic acids in the gas and aerosol phase from photooxidation of 1,3,5-trimethylbenzene in the presence of 300 ppb propene and 300 ppb NOx in smog chamber experiments were determined using a wet effluent diffusion denuder/aerosol collector coupled to ion chromatography (IC) with conductivity detection. Behind the IC, the samples were collected using a fraction collector, for identification of unresolved/unidentified organic acids with IC-mass spectrometry (MS). In total, 20 organic acids were found with MS of which 10 were identified. The organic acids identified offline by IC-MS were then further quantified based on the online IC data. The identification was additionally confirmed with gas chromatography-mass spectrometry. At the maximum aerosol concentration, organic acids comprised 20-45% of the total aerosol mass. The method has a detection limit of 10-100 ng/m3 for the identified carboxylic acids.     

Synthesis of mesoporous nanocrystalline zirconia with tetragonal crystallite phase by using ethylene diamine as precipitation agent

Mesoporous nanocrystalline zirconia with high surface area and pure tetragonal crystallite phase has been prepared by bifunctional ethylene diamine as both precipitating agent for ZrO(NO₃)₂ to ZrO(OH)₂ and colloidal protecting agent for the ZrO(OH)₂ nanoparticles. The effect of refluxing time and temperature on the structural properties of the zirconia were investigated. The obtained results showed that the increasing in refluxing time and temperature improved the thermal stability and increased the tetragonal content of the zirconia. The results also showed that the addition of Pluronic P123 block copolymer surfactant acted as a cosurfactant and increased the specific surface area of the zirconia.     

用气相色谱法对水中有机磷农药的测定

本文采用固相萃取法预处理,然后用带有火焰光度检测器(FPD)的气相色谱仪测定有机磷农药。结果表明,该法具有简单、快速、准确的持点。     

Analysis of n-alkanes in water samples by means of headspace solvent microextraction and gas chromatography

A simple and efficient headspace solvent microextraction (HSME) was developed for the simultaneous determination of the trace concentrations of some n-alkanes in water samples. Therefore, a microdrop of an organic solvent was extruded from the needle tip of a gas chromatographic syringe to the headspace above the surface of the solution in a sealed vial. Then the volatile organic compounds are extracted and concentrated in the microdrop. Next, the microdrop was retracted into the microsyringe and injected directly into the gas chromatograph. Experimental parameters which control the performance of HSME such as the type of microextraction solvent, organic drop and sample volume, sample stirring rate, sample solution and microsyringe needle temperatures, salt addition and exposure time profiles were investigated and optimized. Finally, the enrichment factor, dynamic linear range (DLR), limit of detection (LOD) and precision of the method were evaluated. Using optimum extraction conditions, good linearity with correlation coefficients in the range of 0.995相似文献   

固相萃取-双柱气相色谱法测定水中多种有机磷农药残留

针对单一气相色谱柱定性分析易出现假阳性误判的情况,采用固相萃取-气相色谱双柱技术测定环境水体中多种有机磷农药的残留量。水样中的有机磷农药通过HLB固相萃取小柱富集,经洗脱浓缩后,用DB-35MS和HP-5毛细管气相色谱柱、火焰光度检测器测定。方法的平均加标回收率为86.1%～118%,相对标准偏差为3.2%～6.8%,最低检出限为20～40ng/L,可满足环境水体中痕量有机磷农药残留的分析需要。     

Synthesis of nano titanium oxide with controlled oxygen content using pulsed discharge in water

Different titanium oxide nanoparticles were formed through pulsed discharge of Ti wires in distilled water and H₂O₂ solution. The recovered samples were characterized by various techniques, such as XRD, SEM and TEM. The results confirm the presence of various titanium oxide nanoparticles including TiO₂ phases (anatase and rutile) and various nonstoichiometric TiO_2−x in recovered samples owing to the oxygen deficient circumstance through pulsed discharge. The titanium oxide nanoparticles exhibit a spherical shape with a size of 10–300 nm. The results show that the energy input adjusted by charging voltage is one major factor to control the phases of titanium oxide and the overall oxygen content of recovered samples. In addition, the H₂O₂ content in distilled water also affects the oxygen content of recovered samples. The sample recovered from 10% H₂O₂ solution is pure TiO₂ consisting of anatase and rutile without nonstoichiometric TiO_2−x. Moreover, the UV–Vis absorption spectra of recovered samples show their intensive visible light absorption and the correlation between the visible light absorption and the experimental conditions (charging voltage and H₂O₂ content).     

萃取-水相乙基化衍生结合GC-CVAFS法测定大米和鱼样品中的甲基汞

建立萃取-水相乙基化衍生结合GC-CVAFS测定大米和鱼样品中甲基汞的方法。应用碱消解和有机溶剂CH2Cl2萃取技术,将样品中的甲基汞萃取出来并预富集至水相,而后进行乙基化反应,最后用GC-CVAFS联用系统分离测定。实验结果显示:方法检出限0.001 2 ng/g,萃取前后标准样品回收率分别为97%和95%,精密度RSD均小于5.8%。该方法快速、精密度高、检测限低,能用于环境中痕量甲基汞的检测与分析。     

Determination of tetraethyllead and inorganic lead in water by solid phase microextraction/gas chromatography

A new method for the determination of tetraethyllead (TEL) and ionic lead in water by SPME has been developed. TEL is extracted from the headspace over the sample. Inorganic lead is first derivatized with sodium tetraethylborate to form TEL, which is extracted in the same way as pure TEL samples. The analytical procedure was optimized with respect to pH, amount of derivatizing reagent added, stirring conditions, and extraction time. The detection limit obtained for TEL was found to be 100 ppt when using FID and 5 ppt when using ion trap MS (ITMS). The detection limit for Pb(2+), limited by the nonzero blank, was found to be 200 ppt. Linear calibration curves were obtained for both analytes when FID was used for detection. For lead they spanned over 4 orders of magnitude. ITMS offered excellent sensitivity and selectivity, but the calibration curves were nonlinear when the m/z = 295 ion was used for quantitation. The method has been verified on spiked tap water samples. An excellent agreement was found between the results obtained for standard solutions prepared using NANOpure water and spiked tap water samples.     

Target and nontarget screening of organic micropollutants in water by solid-phase microextraction combined with gas chromatography/high-resolution time-of-flight mass spectrometry

The potential of gas chromatography coupled to high-resolution time-of-flight mass spectrometry (GC/TOF-MS) for screening of organic pollutants in water has been explored. After optimization of the solid-phase microextraction (SPME) step, where parameters such as fiber selection and addition of salt were studied, this extraction technique was applied to the analysis of different types of water samples. Investigation of 60 target organic pollutants, including pesticides, octyl/nonyl phenols, pentachlorobenzene, and polycyclic aromatic hydrocarbons (PAHs) was carried out by evaluating the presence of up to five representative m/z ions per analyte, measured at high mass accuracy, and the attainment of their Q/q (Q, quantitative ion; q, confirmative ion) intensity ratio. This strategy led to the detection of 4-t-octylphenol, simazine, terbuthylazine, chlorpyrifos, terbumeton, and terbutryn in several water samples at low part-per-billion levels. Full spectrum acquisition data generated by the TOF-MS analyzer also allowed subsequent investigation of the presence of polybrominated diphenyl ethers and several fungicides in samples after MS data acquisition, without the need to reanalyze the water samples. In addition, nontarget analysis was also tested by application of a deconvolution software. Several organic pollutants that did not form a part of the list of contaminants investigated were identified in the water samples, thanks to the excellent sensitivity of TOF-MS in full spectrum acquisition mode and the valuable accurate mass information provided by instrument. Bisphenol A, the antioxidant 3,5-di-tert-butyl-4-hydroxy-toluene (BHT), its metabolite 3,5-di-tert-butyl-4-hydroxybenzaldehyde (BHT-CHO), the polycyclic musk galaxolide, and the UV filter benzophenone were some of the compounds present in the water samples analyzed. SPME in combination with GC/TOF-MS has been proved to be an attractive and powerful approach for the rapid screening of multiclass organic pollutants in water, with very little sample manipulation and no solvent consumption. This combination provides to the analyst with information-rich MS data that facilitates the reliable identification of many different organic compounds in samples.