具有阈值电离能力的四极质谱离化器的研制

我们已成功研制出国内第一台具有阈值电离能力的电子轰击电离四级质谱离化器。该离化器电子能量在8．5eV～95eV范围连续可调，电子能量发散半宽度上限为0．5eV。利用该阈值电离技术，我们实现了对N2／CO混合体系中二物种的选择电离及质谱检测。另外，对一些重要气体分子在阈值附近的相对电离截面进行了测定。

Electrochemical oxidation of aniline by a novel Ti/TiO_xH_y/Sb-SnO_2 electrode

Electrochemical oxidation of aniline in aqueous solution was investigated over a novel Ti/TiOxHy/Sb-SnO2 electrode prepared by the electrodeposition method.Scanning electron microscopy,X-ray diffraction,and electrochemical measurements were used to characterize its morphology,crystal structure,and electrochemical properties.Removal of aniline by the Ti/TiOxHy/Sb-SnO2electrode was investigated by ultraviolet-Visible spectroscopy and chemical oxygen demand（COD）analysis under different conditions,including current densities,initial concentrations of aniline,pH values,concentrations of chloride ions,and types of reactor.It was found that a higher current density,a lower initial concentration of aniline,an acidic solution,the presence of chloride ions（0.2wt%NaCl）,and a three-dimensional（3D） reactor promoted the removal efficiency of aniline.Electrochemical degradation of aniline followed pseudo-first-order kinetics.The aniline（200 mL of 100mg·L-（-1）） and COD removal efficiencies reached 100%and 73.5%,respectively,at a current density of 20 mA·cm-（-2）,pH of 7.0,and supporting electrolyte of 0.5 wt%Na2SO4 after 2 h electrolysis in a 3D reactor.These results show that aniline can be significantly removed on the Ti/TiOxHy/Sb-SnO2electrode,which provides an efficient way for elimination of aniline from aqueous solution.

Determination of Iprobenfos Residue in Rice by GC-FTD using Two-dim Ensional Purification

[Objective] This study aimed to establish a determination method for iprobenfos residue in rice straw and husked rice. [Method] The rice straw and husked rice samples were extracted by acetone-ethyl acetate mixed solvent. The extracts were purified using SPE C18 column and SPE NH2 column, and the iprobenfos residues were determined by GC-FTD. [Result] In the concentration range of 0.005-5.0 mg/kg, iprobenfos concentration showed a good linear relationship with peak area （r=0.999 8）. When the iprobenfos concentrations were 0.01, 0.1 and 1.0 mg/kg respectively, the recoveries of added iprobenfos from rice straw ranged from 72.6% to 99.7% with relative standard deviation ranging from 5.65% to 8.48%; the recoveries of added iprobenfos from husked rice ranged from 81.6% to 97.6% with relative standard deviation ranging from 3.74% to 7.63%. The minimum detectable quantity of iprobenfos was 5×10^-12 g, and the minimum detectable concentrations of iprobenfos in rice straw and husked rice samples were 2.0 and 0.5 μg/kg, respec- tively. [Conclusion] The established determination method is characterized by low de- termination limit, high sensitivity, good reproducibility and high operability, which all meet the requirements by Guideline on Pesticide Residue Trials of the Ministry of Agriculture.

Enrichment of carbon recovery of high ash coal fines using air fluidized vibratory deck separator

Coal is primarily beneficiated by wet gravity methods. The wet processing of coal is an efficient practice. However, it introduces the moisture in the range of 6%-15%, depending upon the size of coal which is as detrimental as ash content to the heating value of coal. Dry beneficiation of coal fines was carried out using an air fluidized vibrating table in which the coal particles get separated from the heavier mineral particles as a result of horizontal and vertical stratification. Two level factorial design matrix was used to optimize and assess the interactive effects of the operational parameters of a pneumatic table viz. deck eccentric, side tilt and air flow rate on the clean coal yield and its ash content. Double stage processing was found to be more effective for reducing the ash content of the clean coal. Initial stage of processing at a higher ash level generates a reject of high ash with low combustibles. Cleaning of the rougher concentrate at 34%-35% ash level shows significant improvement in the organic efficiency （88.6%） and useful heat value of clean coal （15690 kJ/kg）. The performance of air fluidized vibrating deck was measured by Ep value which is 0.18.

Effect of the column height on the performance of liquid-solid fluidized bed for the separation of coarse slime

A liquid-solid fluidized bed separator, used for the separation of coarse slime, was developed. Test parti- cles sized in the range from 0.25 to 0.5, 0.5 to 1.0, and 0.25 to 1.0 mm were separated in the liquid-solid fluidized bed. Beds with column heights of 1200, 1500, and 1800 mm were tried. The clean coal and the railings were subsequently analyzed by float-sink testing. The results showed that the ash and yield of clean coal both decreased with increasing column height, for all three size fractions, and that the ash of the clean coal obtained from tests on the broader size fraction was less than that from the narrower sized fractions. The separation density decreased with increasing column height. The lowest E value was seen for a column height of 1500 ram, for which conditions the separation density was 1.45 g/cm3. The E value was 0.084 for the 0.25-0.5 mm fraction but the corresponding separation density was 1.48 g/cm3, and the E value 0.089, for the broader 0.25-1.0 mm fraction.

Supercritical Water as a Reaction Medium for Nitrogen-Containing Heterocycles

Supercritical water has been focused on as an environmentally attractive reaction media, in which organic materials can be decomposed into smaller molecules. The reaction behavior of pyrrole as a simple model compound of nonbasic nitrogen compounds found in petroleum residua was studied in supercritical water with a batch type reactor. The reaction was carried out at temperatures of 698-748 K and at various pressures under an argon atmosphere. The chemical species in the aqueous products were identified by GCMS （gas chromatography mass spectrometry） and quantified using GC-FID （gas chromatography flame ionization detector）. The effect of temperature and reaction time on the conversion process of pyrrole is presented. Under supercritical water conditions, pyrrole underwent successful decomposition in water into its derived compounds. The conversion of pyrrole could approach 81.12 wt% at 723 K and 40 MPa within 240 min of reaction time. The decomposition process was accelerated with the existence of water at the same temperature. Ultimate analysis of solid products was also conducted using a CHN analyzer. The process investigated in this study may form the basis for an efficient method of nitrogen compound decomposition in future.

LONGITUDINAL DISCH.CO_2 LASER WITH PULSED PRE-IONIZATION

A novel pre-ionization scheme of helical transverse-pulsed pre-ionization in a longitudinal discharge CO2 laser is presented. The laser tube is made of glass with inner diameter of 7.5mm and discharge length of 50cm. The laser performance characteristics as functions of parameters, such as pressure, charging capacitance and applied voltage, are investigated. Compared with the same laser structure without pre-ionization, the maximum pulse energy improves by 23%, the optimum electro-optical efficiency increases by 31%, and the specific output energy reaches 26 J/(L·atm).

Biodiesel Production from Waste Cooking Oil by Enzymatic Catalysis Process

Biodiesel is an excellent option for reducing dependence on fossil fuels with environmental advantages by reducing hazardous emissions. The enzymatic transesterification has attracted the attention of researchers in the last decade and the advantages of enzymatic catalysis show that the production of biodiesel by this route has good potential, mainly because it is friendly environment. For biodiesel, production process by enzyme catalysis is chosen the response surface methodology. It is an experimental strategy to find the best operating conditions oftransesterification reaction to improve the biodiesel quality. The Process has three variables： temperature, molar ratio oil-alcohol and catalyst quantity. The process was monitored by GC-FID （gas chromatography with flame ionization detector）. The yield of the transesterification reaction by enzymatic catalysis decreases with increasing temperature, and may be due to inactivation of the enzyme by denaturation at temperatures above 50 ℃. The second-order design used was the ＂CDC （central design composition）＂ which produced a maximum yield of 95.5% in the transesterification reaction by enzymatic catalysis obtained at a temperature of 45 ℃, molar ratio methanol：oil of 8：1 and a catalyst loading of 8% wt.

Numerical Simulation of Fluid Flow and Oil-Water Separation in Hydrocyclones

The fluid flow and oil-water separation were simulated using a Reynolds stress transport equation model of turbulence in water flow and a stochastic model of oil droplet motion. Simulation results give the axial and tangential velocity components, the pressure and turbulence intensity distribution and droplet trajectories for a hydrocyclone of F type and a hydrocyclone proposed by the present authors. The flow field predictions are in qualitative agreement with the LDV measurements. The results show that the proposed hydrocyclone has better performance than the hydrocyclone of F type due to creating stronger centrifugal force and lower axial velocity.

Experimental and Theoretical Study of Reactions between Manganese Oxide Cluster Cations and Hydrogen Sulfide

Manganese oxide cluster cations Mnm180n＋ were prepared by laser ablation and reacted with hydrogen sulfide （H2S） in a fast flow reactor under thermal collision conditions. A time-of-flight mass spectrometer was used to detect the cluster distributions before and after the interactions with H2S. The experiments suggest that oxygen-for-sulfur （O/S） ex- change reaction to release water took place in the reactor for most of the manganese oxide cluster cations： MnmlSOn＋＋H2S→Mnm18On-1S＋＋H218O. Density functional theory cal- culations were performed for reaction mechanisms of Mn202＋＋H2S, Mn203＋＋H2S, and Mn204＋＋H2S. The computational results indicate these O/S exchange reactions are both thermodynamically and kinetically favorable, thus in good agreement with the experimental observations. The O/S exchange reactions identified in this gas-phase cluster study parallel similar behavior of related condensed phase reaction systems.

Triboelectrostatic Separation-an Efficient Method of Producing Low Ash Clean Coal

At present, coal is mainly consumed as fuel. In fact, coal is also a kind of precious raw material in chemical industry on the premise that some harmful minerals should be removed from coal. The paper presents the results of the research on producing low ash (<2%) coal with triboelectrostatic separator used for producing high-grade active carbon. The test is conducted in bench-scale system, whose capacity is 30～100 kg/h. The results indicate that: 1) the ash content of clean coal increases with the increase of solid content of feedstock, on the contrary, the yield of clean coal is declining; 2) a high velocity may result in a good separation efficiency; 3) for the same solid content, the reunion caused by intermolecular force makes the separation efficiency drop down when the ultra-fine coal is separated; 4) the separation efficiency is improved with the increase of electric field intensity, but there is a good optimized match between the electric field intensity and yield of clean coal; 5) a low rank coal is easy-to-wash in triboelectrostatic separation process; 6) the yield of clean coal can be enhanced and the ash decreased through adapting optimized conditions according to various coals.

Constitutive Model for Multiaxial Ratcheting Predictions of Cyclic Softening Weld Metal

A series of fully reversed axial, torsional strain-controlled cyclic tests and two multiaxial ratcheting tests were conducted on weld metal specimens using an Instron8521 tension-torsional servo-controlled testing machine. The weld metal showed clear cyclic softening under axial, torsional and multiaxial loading. A modified kinematic hardening rule was proposed in which a multiaxial-loading-dependent parameter incorporated the radial evanescence term of the Burlet-Cailletaud mode with the Ohno-Wang kinematic hardening rule to predict the multiaxial ratcheting effects. The introduction of yield stress evolved with accumulated plasticity strain enables the model to predict cyclic plasticity behavior of cyclic softening or cyclic hardening materials. Thus modified model considers the isotropic hardening as well as kinematic hardening of yield surface, and it can present description of plasticity behavior and ratcheting of cyclic softening and cyclic hardening materials well under multiaxial loading.

Enhanced heat transfer in a heat exchanger square-duct with discrete V-finned tape inserts

The article presents an experimental and numerical study on thermal performance enhancement in a constant heatfluxed square-duct inserted diagonally with 45° discrete V-finned tapes(DFT).The experiments were carried out by varying the airflow rate through the tested square duct with DFT inserts for Reynolds number from 4000 to 25000.The effect of the DFT with V-tip pointing upstream at various relative fin heights and pitches on heat transfer and pressure drop characteristics was experimentally investigated.Both the heat transfer and pressure drop were presented in terms of Nusselt number and friction factor respectively.Several V-finned tape characteristics were introduced such as fin- to duct-height ratio or blockage ratio(R_B=e/H = 0.075,0.1,0.15 and 0.2),fin pitch to duct height ratio(R_P= P/H=0.5,1.0,1.5 and 2.0) and fin attack angle,α = 45°.The experimental results reveal that the heat transfer and friction factor values with DFT inserts increase with the increment of R_B but the decrease of R_P.The inserted square-duct at R_B = 0.2 and R_P = 0.5 provides the highest heat transfer and friction factor while the one with R_B= 0.1 and R_P= 1.5 yields the highest thermal performance.Also,a numerical simulation was conducted to investigate the flow structure and heat transfer mechanism inside the tested duct with DFT inserts.

Conversion of Methane by Steam Reforming Using Dielectric-barrier Discharg

Conversion of methane by steam reforming was carried out by means of dielectric-barrier discharge.A systemic procedure was employed to determine the suitable experimental conditions.It was found that one of the plasma generators can match the system best.A higher power input can always bring a higher conversion,but the selectivity to C2H6 decreased from 52.48% to 39.43% as the power increased from 20W to 49W.When discharge distance was 4mm,selectivities to almost all main products reached the max.The inner electrode made of stainless steel and the outer electrode with aluminum foil were one of the best options which can obviously enhance the conversion of methane.A larger flow rate always resulted in a lower conversion of methane.In the most time,19.93% steam promoted conversion of methane.

Pressure Oxidative Leaching of Complex Sulphide Concentrate

The presented results are related to the leaching of Pb-Zn-Cu-Fe sulphide concentrate, obtained from barite-sulphide ores, under the elevated temperatures and pressures in an autoclave. The leaching process was performed using the sulphur acid solution with the oxygen addition for the separation of the targeted metals from the polymetallic concentrate. In this process influences of various parameters were discussed and then correlated to the leached metals, zinc, copper and iron. Zinc, copper and iron were dissolved in a solution, while lead remained as insoluble in the leach residue. The best leaching results were determined under the temperature of 210 ℃ during the 240 min. Obtained leaching degrees were 98% zinc, 95% copper and 96% iron.

Phytochemical Screening of Essential Oil of Citrus sinensis by Gas Chromatography-Flame Ionization Detector

Citrus sinensis commonly called sweet orange belongs to the family Rutaceae. Nutritionally, it is highly recommended due to its high content of micronutrients. However, the rejection of a large amount of epicarp in nature contributes to the emission of greenhouse gas and the development of leachate which contaminate surface water and groundwater. The aim of this work was to identify the essential oil components from Citrus sinensis epicarp, and then look after the biological activity of these components in order to underline the worth to reuse the Citrus sinensis epicarp as a gainful mean. The essential oil of 4,000 g of Citrus sinensis epicarp was done through the water steam distillation and 0.0287 g of essential oil was obtained; so a yield of 0.0007%. The essential oil was then submitted to gas chromatography-flame ionization detector （GC-F1D）. The result revealed that the essential oil was teemed with 28 volatile compounds, including terpene compounds （50%）, aldehydes （32%） and alcohols （18%） whose anti-inflammatory, anti-diabetic, larvicidal and antioxidant activities were underlined.

Commissioning of Commercial Scale Pressure Filter Test Facility of PTA Unit at Yangzi Petrochemical Co.

The Yangzi Petrochemical Company has successfully imple-mented the test commissioning of a 45 t/h pressure filter (base on dry feed material) installed in the PTA unit with its pressure filter technique commanding a leading

Hydrothermal synthesis and energy storage performance of ultrafine Ce2Sn2O7 nanocubes

Ultrafine cube-shape Ce2Sn2O7 nanoparticles crystallized in pure pyrochlore phase with a size of about 10 nm have been successfully synthesized by a facile hydrothermal method.Conditional experiments have been conducted to optimize the processing parameters including temperature,pH,reaction duration,precipitator types to obtain phase-pure Ce2Sn2O7.The crystal structure,morphology and sizes and specific surface area have been characterized by X-ray diffractometer(XRD),Raman spectrum,transmission electron microscope(TEM),high resolution transmission electron microscope(HRTEM),and Brunauer-Emmett-Teller(BET).The as-synthesized Ce2Sn2O7 ultrafine nanocubes have been evaluated as electrode materials for pseudo-capacitors and lithium ion batteries.When testing as supercapacitors,a high specific capacitance of 222 F/g at 0.1 A/g and a good cycling stability with a capacitance retention of higher than 86%after 5000 cycle have been achieved.When targeted for anode material for lithium ion batteries,the nanocubes deliver a high specific reversible capacity of more than 900 mA·h/g at 0.05C rate.The rate capability and cycling performance is also very promising as compared with the traditional graphite anode.

Structural Optimization of a Novel Up-run Gas-solid Separator

A new gas-solid separator dedicated to heavy-oil fast pyrolysis process incorporating inertial and centrifugal separation was designed. Gas and typical fluid catalytic cracking （FCC） catalyst particles （with a density of 1500 kg/m3, and a mean diameter of 45.81 p.m） were used in the study. The inlet gas velocity was kept constant at 13.36 m/s, while the solid loading at the inlet ranged from 0 to 700 g/m3. When the exhaust pipe opening was provided with two narrow-width slots near the inlet without baffles, the solid collection efficiency increased with an increasing solid loading at the inlet and was close to 95% along with a decreasing pressure drop. After increasing the secondary separation structure, the separation efficiency greatly improved. By adjusting the diameter of the secondary exhaust pipe, the separation efficiency and pressure drop could be balanced. Under the experimental conditions, when the diameter of the second exhaust pipe was equal to d=100 mm, the pressure drop was lower than 1400 Pa while the separation efficiency could exceed 99.50%; and when the diameter was equal to d=120 mm, the pressure drop was less than 700 Pa, with the separation efficiency reaching over 99.00%.

The role of the symmetry and the flexibility of the anion on the characteristics of the nanostructures and the viscosities of ionic liquids

The transport properties of ionic liquids(ILs) are crucial properties in view of their applications in electrochemical devices. One of the most important advantages of ILs is that their chemical–physical properties and consequently their bulk performances can be well tuned by optimizing the chemical structures of their ions. This will require elucidating the structural features of the ions that fundamentally determine the characteristics of the nanostructures and the viscosities of ILs. Here we showed for the first time that the "rigidity", the order,and the compactness of the three-dimensional ionic networks generated by the anions and the cation head groups determine the formation and the sizes of the nanostructures in the apolar domains of ILs. We also found that the properties of ionic networks are governed by the conformational flexibility and the symmetry of the anion and/or the cation head group. The thermal stability of the nanostructures of ILs was shown to be controlled by the sensitivity of the conformational equilibrium of the anion to the change of temperature. We showed that the viscosity of ILs is strongly related to the symmetry and the flexibility of the constitute ions rather than to the size of the nanostructures of ILs. Therefore, the characteristics of the nanostructures and the viscosities of ILs, especially the thermal stability of the nanostructures, can be fine-tuned by tailoring the symmetry and the conformational flexibility of the anion.