Volume 34,Issue 7,2011 Table of Contents

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  • 1  The input load and its influence factors of wind turbine based on variational wind speed
    QIN Da-tong LI Qi
    2011, 34(7):1-7. DOI: 10.11835/j.issn.1000-582X.2011.07.001
    [Abstract](2325) [HTML](0) [PDF 8.62 M](1442)
    Abstract:
    The auto regressive (AR) method is applied to build the model of wind speed in wind field,and with the model, the wind time-history is obtained. The Glauert method is used to calculate time-varying input load,such as the time histories of thrust and torque of the wind turbine under the condition of variational wind speed. Based on statistical analysis,the design loading spectrum and rain flow histogram of the loads are obtained. The effects of wheel blade parameters on the input load under the condition of variational wind speed are analyzed,and the average loads of thrust and torque are obviously affected by the pitch angle. When the pitch angle increases,the loads of thrust and torque both decrease,meanwhile the amplitude of thrust first increases then decreases,while the amplitude of torque decreases monotonously. The thrust is obviously affected by twist and attack angles of blade while the torque is less affected by the twist and attack angles of the blade. The results lay foundations for reliability design,load control of the wind turbine as well as the parameter optimum of the wheel blade aerofoil under the real wind condition.
    2  Deformation analysis of engines’ connecting-rods including oil film forces reconstructed by RBFNN
    MENG Fan-ming
    2011, 34(7):8-13. DOI: 10.11835/j.issn.1000-582X.2011.07.002
    [Abstract](1632) [HTML](0) [PDF 7.24 M](1163)
    Abstract:
    A coupling analysis method is proposed for the transient deformation of engines’ connecting-rods. A radial base function neural network (RBFNN) with three layers is designed to reconstruct the two-dimensional oil film forces. Forces acting on the two ends of the connecting-rod are achieved through coupling equations for it. Further,finite element analyses of transient deformation for the connecting-rod are made through software ANSYS. Meanwhile,the validity of the proposed method is demonstrated. Numerical results show the maximum deformation of a rotary connecting rod occurs before or behind the bottom dead center at compression stroke when the two-dimensional oil film forces are considered.
    3  The application of functional theory to the design of new wind turbine blades
    CHEN Jin ZHANG Shi-qiang LU Qun-feng CHENG Jiang-tao
    2011, 34(7):14-19. DOI: 10.11835/j.issn.1000-582X.2011.07.003
    [Abstract](2560) [HTML](0) [PDF 7.91 M](2343)
    Abstract:
    Considering the tip loss of normal and tangential forces,a new aerodynamic model of wind turbines is given. Based on the new series of dedicated high-performance wind turbine airfoil,the functional expressions of wind turbine blade chord and twist angle span-wise distribution are studied,and then a new common functional equation of the blade shape is presented. Considering the wind farmer wind speed distribution,air density and industrial requirements of the wind turbine blade,aiming at the maximizing annual energy generation in constant and variable speed operation condition respectively,assigning the coefficients of blade distribution functions as the variables,a 2.3 MW wind turbine blade shape optimization model is established. Two kinds of superior blade are also optimized. The efficiency and the annual electricity production of the new blades are much higher than traditional blades. Among the new blades,the maximum power coefficients of fixed speed blade and variable speed blade are 0.515 7 and 0.517 7 respectively.
    4  Design calculation and finite element simulation analysis of stranded wire helical springs
    XIAO Hong WANG Shi-long ZHOU Jie FENG Zhi-heng LEI Song
    2011, 34(7):20-27. DOI: 10.11835/j.issn.1000-582X.2011.07.004
    [Abstract](1923) [HTML](0) [PDF 9.46 M](1435)
    Abstract:
    The spatial structure of single wire is analyzed based on the forming process of stranded wire helical springs. Additionally,three parameters are derived from the existing foundation,including distribution circle radius of strand,spiral parameter of single wire and track scanning parameter. The aided design method of stranded wire helical springs based on feature scanning is put forward in which the centerline model of single wire can be obtained through one scanning step and the modeling method is given based on PROE code. The simulation analysis for spring in loading is performed by using ABAQUS code based on the calculation results. The finite element analysis results show the stress-strain ability of wire and the stress distribution of the section. The affects of loading rate on vibration of coils is also found.The results can make up for the deficiency of existing methods and give more beneficial assistance for production processing and performance test of the stranded wire helical springs.
    5  Efficiency optimization matching strategy of continuously variable transmission system with reflux power
    YIN Yan-li SUN Dong-ye LIN Xin-you HAO Yun-zhi
    2011, 34(7):28-33. DOI: 10.11835/j.issn.1000-582X.2011.07.005
    [Abstract](2500) [HTML](0) [PDF 9.66 M](1075)
    Abstract:
    To solve the problem that the transmission efficiency of continuously variable transmission system with reflux power varies in a great range, and the traditional control strategy can’t make sure that the overall system is under ideal conditions, an economy control method based on system efficiency optimization is put forward. The engine/transmission efficiency numerical model and system optimization model are built. Taking Matlab/Simulink as the platform, objective throttle position control table and objective ratio control table are obtained by solving the optimization model. Furthermore, ECE+EUDC drive cycle simulation based on the fuel economy of sample car is carried out, and the simulation results indicate that the method of system efficiency optimization make fuel consumption reduce by more than 1.5%.
    6  Preparation of TiFe alloy by electro-deoxidization in molten calcium chloride from titanium concentrates
    SHI Rui-meng BAI Cheng-guang DU Ji-hong
    2011, 34(7):34-38. DOI: 10.11835/j.issn.1000-582X.2011.07.006
    [Abstract](2014) [HTML](0) [PDF 5.89 M](918)
    Abstract:
    TiFe alloy is prepared by the electrolytic reduction of molten-solidified titanium concentrate in molten CaCl2, which is obtained under argon atmosphere. The formation mechanism of TiFe alloy is discussed. The impact of electrolyte time on product is studied when electrolyte voltage is 3.1 V and electrolyte temperature is 900 ℃. Research results show that TiFe alloy with uniform composition can be obtained by this means. The deoxidize product is iron and TiFe alloy by order. The reduction of Ti is a multi-step process and the intermediate products include CaTiO3, TiO2, Ti2O3, TiO, Fe and TiFe2.
    7  Simulation method for multi-machine and multi-task crane scheduling in steelmaking plant
    CHEN Kai ZHENG Zhong ZHOU Chao
    2011, 34(7):39-45. DOI: 10.11835/j.issn.1000-582X.2011.07.007
    [Abstract](2177) [HTML](0) [PDF 7.87 M](1503)
    Abstract:
    It is of great significance in steel complex to link production flow between work stations and control production rhythm by cranes. Crane scheduling is a multi-machine multi-task problem which limits temporal and spatial constraints and production plan. A simulation model based on evolution rules to solve temporal and spatial constraints is proposed. Its objective is to guarantee execution of production plan in steelmaking plant. And match between cranes and production task on working span is conducted to fulfill temporal constraints between multi-tasks and spatial constraints among multi-cranes. Simulation rules including task allocation, conflicts eliminating and task finishing are also proposed to dominate simulation process. This model avoids difficulties of theoretical calculation for crane scheduling problem. Offline test in a steelmaking plant shows that it is available to make a crane scheduling without conflicts between cranes and plans, which provides a guideline for production scheduling.
    8  Numerical simulation and experimental investigation of double-stage sheet incremental forming
    ZHOU Jie HU Jian-biao ZHANG Xu LI Jun-chao
    2011, 34(7):46-50. DOI: 10.11835/j.issn.1000-582X.2011.07.008
    [Abstract](2136) [HTML](0) [PDF 6.38 M](1543)
    Abstract:
    In order to find a method to reduce excessive sheet thinning in the forming process of small half-apex angle parts by incremental sheet forming, a finite element model (FEM) for simulating double-stage process is developed in ABAQUS. Then, the simulation results, such as sheet thickness distribution and equivalent plastic strain history, are compared with those of single-stage simulation. The effects of double-stage on formability of sheet are discussed. The results show that using double-stage process instead of single-stage in forming parts, the maximum deformation is nearer to the parts’ bottom surface, and the maximum equivalent plastic strain of node A, B, C is reduced by 66.2%, 81.9% and 36.0% respectively. The sheet thickness is better distributed, and the minimum thickness increases by 16%. In addition, double-stage incremental forming can greatly improve the formability of sheet. The simulation results are in a good agreement with experimental results.
    9  Effect of different temperatures and strain rates on the critical damage factor of 7075 aluminum alloy
    QUAN Guo-zheng WANG Yi-xin ZHANG Yan-wei WANG Feng-biao GAO Lin
    2011, 34(7):51-56. DOI: 10.11835/j.issn.1000-582X.2011.07.009
    [Abstract](1972) [HTML](0) [PDF 7.26 M](1996)
    Abstract:
    The computation principle of Cockroft-Lathem ductile cumulative damage is analyzed. A method to solve the critical damage factor based on the evolution rules of damage sensitive rate is brought forward. Several series of billet samples are compressed on heat physical simulation machine under different deformation temperatures and strain rates, and then the collected true stress-strain data are used to calculate the performance of computations. As the outer edge of upsetting drum where the maximum damage value appears is concerned, a typical damage softening rule is obtained and described as the damage sensitive rate decreases rapidly at the initial deformation, then gradually tends to 0. In further, damage softening is more sensitive to strain rate than temperature. A principle that critical damage factor arises when damage sensitive rate decreases to 0 is assumed, then the distribution of critical damage factor under temperature 573~723 K and strain rate 0.01~10 s-1 is obtained. The results show that the critical damage factor of 7075 aluminum alloy is not a constant but a change within a range of 0.255 ~ 0.453, and it is more sensitive to strain rate in high temperature and more sensitive to temperature in high strain rate.
    10  The design of torque dynamic sliding mode controller in permanent magnet synchronous generator for wind turbine
    HU Xue-song SUN Cai-xin LIAO Yong ZHUANG Kai
    2011, 34(7):57-62. DOI: 10.11835/j.issn.1000-582X.2011.07.010
    [Abstract](1879) [HTML](0) [PDF 7.55 M](1055)
    Abstract:
    Permanent magnet synchronous generator for wind turbine is a multivariable nonlinear system with strong coupling. Considering the influence of the volatile parameters of the generator on the performance of vector control, the torque dynamic sliding-mode control strategy is further studied. The proposed first order dynamic sliding-mode control strategy reduces the chattering by using a new switch function constituted with derivative element. With the dynamic sliding-mode controller in the power outer loop, the PMSG vector control system shows excellent robustness and insensitivity to the parameters and disturbance, which is confirmed by simulation.
    11  Overall control strategy and operational performances of a doubly fed wind turbine generator system
    ZHANG Zhi-jun LI Hui CHEN Hong-wen YANG Chao TANG Xian-hu
    2011, 34(7):63-68. DOI: 10.11835/j.issn.1000-582X.2011.07.011
    [Abstract](1939) [HTML](0) [PDF 7.26 M](1280)
    Abstract:
    In order to comprehensively and correctly analyze the real-time operational characteristics of a grid-connected wind turbine generator system, it is necessary to analyze the overall control strategies and operation performances of the wind turbine generator system. According to the type of a doubly fed wind turbine generator system, the mathematical models of wind turbine, drive train and doubly fed induction generator (DFIG) are presented. From the viewpoints of the maximum wind energy capture and safe operation of the wind turbine, a maximum power output control strategy is proposed by considering the DFIG loss minimization, and a variable pitch control strategy is also presented by considering generator rotational speed restriction and the output power restriction. Combined with a power decoupling strategy of DFIG, the overall operational performances of the doubly fed wind turbine generator system are simulated. By comparing the simulation, theoretical analysis and actual operational data, the results show that the presented model and overall control strategies of the doubly fed wind turbine generator system are valid.
    12  AC icing flashover performance of 110 kV potential transformer and the measures of anti-icing flashover
    ZHANG Zhi-jin JIANG Xing-liang HU Jian-lin CHEN Ling LIU Bing HUANG Hai-zhou
    2011, 34(7):69-75. DOI: 10.11835/j.issn.1000-582X.2011.07.012
    [Abstract](2916) [HTML](0) [PDF 7.42 M](1049)
    Abstract:
    The AC flashover performance of 110 kV iced potential transformer is investigated by testing in laboratory to analyze the influence degree of icing on the safe and reliable operation of power system. The results show that the AC flashover voltage of 110 kV iced potential transformer decreases with the ice amount increasing. The relation between icing flashover voltage and ice amount accords with the negative exponential function law, and the characteristic index is in the range of 0.085~0.100. Meanwhile, the relation between icing flashover voltage and ice thickness accords with the negative power function law, and the characteristic index is in the range of 0.40~0.55. The flashover voltage of 110 kV iced bushing is related to the pollution before icing. The relation between icing flashover voltage and salt deposit density (SDD) accords with the negative power function law, and the characteristic index is in the range of 0.21~0.26. When the ice thickness is up to 25 mm and SDD is 0.08 mg/cm2 and above, the icing flashover occurs on the 110 kV potential transformer in service. The effective measures to prevent AC icing flashover of 110 kV potential transformer are to increase the height of the structure and install creepage extenders. The results can offer consults for the external insulation selection and design of substation in ice covered regions.
    13  Wavelet denoising method of temperature signal in the process of coal gas absorption and desorption
    XU Jiang WU Xin PENG Shou-jian YANG Hong-wei
    2011, 34(7):76-82. DOI: 10.11835/j.issn.1000-582X.2011.07.013
    [Abstract](1877) [HTML](0) [PDF 9.11 M](1410)
    Abstract:
    The study on the temperature evolutionary trend under both the ground stress and gas pressure is significant in the process of coal gas absorption and desorption. However, the valid signal is difficult to gain because of much noise in the experimental data, so according to the characteristics of the temperature signal gained under different experimental conditions of coal gas absorption and desorption, this essay filtrates noise and restores the valid signal by using the wavelet denoising of MATLAB to obtain the valid temperature evolutionary curve. Through contrasting and analyzing wavelet basis function and different decomposition levels, the essay chooses the sym8 wavelet basis function which has a higher order of vanishing moments and better smoothness. The reconstructed signal filtrates most of high frequency signal, and keep low frequency, as well as smooth signal. The result shows that the de-noising effect is good and the temperature evolution rule can be well reflected in the process of the coal gas absorption and desorption.
    14  Numerical simulation of carbon dioxide storage in unmineable coalbed
    ZHOU Jun-ping XIAN Xue-fu JIANG Yong-dong LIU Zhan-fang
    2011, 34(7):83-90. DOI: 10.11835/j.issn.1000-582X.2011.07.014
    [Abstract](2285) [HTML](0) [PDF 9.04 M](1100)
    Abstract:
    The injection of carbon dioxide (CO2) in deep unmineable coalbeds(CO2-ECBM) is a very attractive option for geologic CO2storage. The CO2 is stored and at the same time the recovery of coalbed methane is enhanced. The revenue of methane (CH4) production can offset the expenditures of the storage operation. The processes involving in the CO2-ECBM include multi-components gas adsorption,diffusion,and gas-water two phase flow in coalbed. On the basis of above processes,a model considering adsorption induced coal matrix swelling is developed, which can be used to describe multi-components gas adsorption/desorption-diffusion-flow in coalbed. The finite difference method is used to solve this model,and the comparison of the results with the existed model suggests the model is valid. Then the model is applied to evaluated the influence of permeability of coal seam,different gas adsorption induced swelling,CO2/CH4 adsorption capacity ratio,pore model considering matrix swelling,and gas composition of injection gas on CO2 sequestration and methane production, and these results are very important for site selection and technological parameters optimum of CO2-ECBM project.
    15  Experiments of coal’s gas seepage with outburst dangers
    CAO Shu-gang BAI Yan-jie LI Yong GUO Ping LIU Yan-bao
    2011, 34(7):91-95. DOI: 10.11835/j.issn.1000-582X.2011.07.015
    [Abstract](1895) [HTML](0) [PDF 5.63 M](1261)
    Abstract:
    The experiments of outburst coal’s gas seepage are carried out by triaxial permeameter which is independently developed. Under the condition of fixed gas pressure, different confining pressures and axial pressures acting on raw coal test samples are tested. It shows that as the increasing of confining pressure, coal sample seepage velocity tends to decline, and this phenomenon is more obvious for the coal with serious original injury. The relationship between seepage velocity and confining pressure can be described as a quadratic function,and its general expression is established. Coal sample’s seepage velocity-strain path is similar to stress-strain path, therefore, the changes in coal seepage velocity indirectly reflects the process of the evolvement of coal damage. The influence of effective stress on coal sample seepage velocity can be concluded as hypersensitive stage and smooth stage, and in the hypersensitive stage, seepage velocity of the coal sample vary quickly, while in smooth stage, its variety is not obvious. In different stress conditions, the degree of development for hole and cranny of coal affect coal gas energy and elastic deformation energy in coal body as well as the form of coal destruction.
    16  Synthesis of cationic polyacrylamide usinginverse emulsion polymerization
    ZHENG Huai-li WANG Wei JIANG Shao-jie SHEN Lie-xiang LIU Lan ZHANG Hui-qin FAN Wei
    2011, 34(7):96-101. DOI: 10.11835/j.issn.1000-582X.2011.07.016
    [Abstract](2512) [HTML](0) [PDF 5.89 M](1202)
    Abstract:
    The cationic polyacrylamide is synthesized by acrylamide (AM) and propenoyl-ethyl trimethyl ammonium chloride (DAC) through inverse emulsion polymerization, using liquid paraffin as continuous phase and Span80-Tween80 as compound emulsifier. The influence factors for the viscosity of product and the stability of the system are discussed, such as the ratio of oil to water, emulsifier dosage, monomer dosage, cationic degree and initiator dosage. When the volume ratio of oil to water is 1∶1.6, the emulsifier dosage is 30%, the monomer dosage is 30%, the cationic degree is 60%, i.e. the molar ratio of AM to DAC is 2∶3, and the initiator dosage is 0.15%, the obtained product has high viscosity and stability. The effects of viscosity and polymer dosage on flocculating are studied in flocculating experiment, and the polymer structure is analyzed by IR spectrum.
    17  Analysis on wall slip phenomenon andcharacteristics of sewage sludge
    FENG Min-quan ZHANG Li ZHANG Xiao-bin Hansong TANG
    2011, 34(7):102-106. DOI: 10.11835/j.issn.1000-582X.2011.07.017
    [Abstract](1593) [HTML](0) [PDF 7.09 M](1152)
    Abstract:
    Wall slip of sewage sludge and possible slip in fluencing factors are studied experimentally by using a rotational rheometer with parallel plate fixtures and by high speed camera.The technique involves placing a straight line marker to monitor wall slip, checking the gap dependence of the stress-strain data and studying the time-stress data trend of strain stepped scanning. In the shearing flow it is found that, for sewage sludge of water content 80%, as the strain amplitude increases, the stress data starte to diverge at a certain strain amplitude, indicating that wall slip occurs. Meanwhile, it has been utilized for studying the critical shear stress and calculating the slip velocity, and the formulation of shear stress and slip velocity are fitted. But for sewage sludge of water content 90%, these curves are superimpose, indicating no slip occurs.While scanned sewage sludge water content 80% at different shear rates in 5 s and 60 s, it is found that under 5 s and 60 s, when the shear rate is greater than 10 s-1 and 0.5 s-1 respectively, peak appeas in time-stress curves, i.e. slip occurs. Therefore, concentration, shear rate and time have influence on wall slip.
    18  A study on the incineration product and reaction process of TFT liquid crystal
    GUO Yu-wen LIU Jing-yang QIAO Qi LIANG Ji-jun ZHANG Jian-qian
    2011, 34(7):107-113. DOI: 10.11835/j.issn.1000-582X.2011.07.018
    [Abstract](2297) [HTML](0) [PDF 7.79 M](1346)
    Abstract:
    The incineration reaction process of TFT liquid crystal is speculated according to the weight loss character and analysis results of incineration production. It is indicated that the 90% weight is loss from 150 ℃ to 380 ℃ in the incineration process of TFT liquid crystal, which is composed of some monomer compounds. Decomposition reaction first occurs in the process of incineration process. The order of decomposition product lies on the chemical bond energy of monomer compound. The production of radical alkyl and radical aromatic in decomposition process are unstable. Radical alkyl is decompounded hydrocarbon that has much less carbon atom, such as propylene. Decomposition reaction of radical aromatic continues and defluorinate happens with temperature rise. The synthesize reaction occurs between the decomposition production. The production is admixture composed of different aromatic compounds in low temperature. PAHs and HF are observed in high incineration temperature. The mostly incineration production of TFT liquid crystal are venomousness and injurant, so it is not suitable to treat TFT liquid crystal with incineration.
    19  Dynamics of nitrogen and phosphorus in paddy field under deep application condition of urea pill and its pollution-reducing potential
    FENG Guo-lu GONG Jun-hui
    2011, 34(7):114-119. DOI: 10.11835/j.issn.1000-582X.2011.07.019
    [Abstract](1703) [HTML](0) [PDF 7.42 M](1173)
    Abstract:
    Dynamics of the pollutants such as nitrogen, phosphorus and the suspended particulates in the field water and soil and its pollution-reducing potential are investigated in the rice plant returning-green stage using deep application technique of urea pill with the application depth of 3, 7 and 11 cm (expressed as t-3, t-7 and t-11, respectively) based on the micro-zone simulation field experiments. Results show that nitrogen content in the field water gradually decreases within 5~7 d after deep allocation of urea, and reaches the low level after the seventh day. NO-3-N concentration is higher than NH+4-N, but there is little difference between treatments. As the pollution source is concerned, NO-3-N in the field water should be considered. There isn’t any correlation between nitrogen content in the water and urea application depth in the field. By contrast with blank treatment(expressed as t-c), NO-3-N, NH+4-N and TN contents in the field water with deep application of urea pill decrease 29%~47%, 64%~89% and 79%~97%, respectively. The TP and DP are in the high level in the field water with t-3 and t-7. The TP, DP and SS concentration in the field water with t-11 decrease 32%~73%, 92%~99% and 50%~80%, suggesting that deep application of urea pill into 11 cm layer of the field should have a significant pollution-reducing potential and become one of effective measures to control non-point source pollution of agricultural system.
    20  The experiments on surface modification activated carbon for the removal of 2,4,6-trichlorophenol from water
    ZHAN Jian ZHU Dong-mei LIU Zhen-zhong
    2011, 34(7):120-124. DOI: 10.11835/j.issn.1000-582X.2011.07.020
    [Abstract](1406) [HTML](0) [PDF 5.65 M](1189)
    Abstract:
    Surface of granular activated carbon modified by Fe and Mn is used in the experimental study of dynamic adsorption of 2,4,6-trichlorophenol(TCP) in water. It is showed that the adsorption effect of 2,4,6-trichlorophenol with granular activated carbon modified by Fe and Mn is affected by initial water concentration, initial pH value and flow rate, etc. In addition, to recycle granular activated carbon modified by Fe and Mn, it is oscillated with NaOH solution (mass fraction is 4%) in oscillator at 10 ℃ for 24 h. It is found that the adsorption capability is still good after three times of regeneration.
    21  Effect of thermal radiation on thermal flow field in inclined tunnel
    HUO Yan GAO Ye WU Hong-mei ZOU Jian-feng
    2011, 34(7):125-130. DOI: 10.11835/j.issn.1000-582X.2011.07.021
    [Abstract](1441) [HTML](0) [PDF 7.83 M](1011)
    Abstract:
    The thermal radiation is the main factor affecting internal thermal flow field in a tunnel. This paper studies on two open ends of a channel inclined with angles of 10°, 20° and 30° by experiments and numerical simulations. The experimental data agree well with the predicted results by using Large Eddy Simulation (LES) to solve N-S equations driven by the buoyancy flow. And the influence of thermal radiation on thermal flow field of tunnel with inclination angles from 10° to 30° at same heat source is obtained by comparing the experiment results and numerical resolutions of coupled with radiation model and without radiation model. Thermal radiation makes temperature near the upper wall of tunnel drop, and the influence of thermal radiation on bottom end of tunnel declines with the inclination angle increasing. However, the inclination angle has a little effect on temperature near the ceiling of the top end of tunnel. Simultaneously, the higher temperature zone leaning to the top end due to the thermal radiation is obtained, and the temperature at the bottom of the upper part of the tunnel increases. The findings of the study are important references for theory research of thermal flow field in inclined tunnels.
    22  Simultaneous determination of multiple organophosphorus pesticides residues in honey by liquid chromatography tandem mass spectrometry
    WANG Guo-min LI Ying-guo DAI Hua XIE Wen ZHANG Jin-zhong ZHOU Qi-ming LI Zheng-guo
    2011, 34(7):131-136. DOI: 10.11835/j.issn.1000-582X.2011.07.022
    [Abstract](2603) [HTML](0) [PDF 6.07 M](1385)
    Abstract:
    The trichlorfon, dichlorvos, and coumafos are commonly used as organophosphorus pesticides to control pests or natural enemies of bees, but they easily contaminate the honey. A simultaneous determination method for trichlorfon, dichlorvos and coumafos residues in honey is developed by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Samples are extracted with ethyl acetate and concentrated extracts, and then the residue is dissolved by methanol, and separated by HPLC, detected by electrospray ionization (ESI)-MS/MS with multiple reaction monitoring mode (MRM). It is found that the linear ranges of the three organophosphate pesticides are 20~500 μg/L with correlation coefficients over 0.994, the detection limits (LODs) are 0.1 μg/kg and the limits of quantification (LOQs) are 4 μg/kg for all of the three pesticides. The average recoveries of the three pesticides in spiked honeies at concentration levels of 10~40 μg/kg range from 78.5% to 96.8%, and the relative standard deviations are in the range of 9.1%~13.1%.
    23  Interference elimination of PCB and its ramification in determining trace PBBs/PBDEs by GC/MS
    HUA Liab ZHANG Hong-quan ZHANG Lei LIU Tao HUANG Yuan-qiao
    2011, 34(7):137-146. DOI: 10.11835/j.issn.1000-582X.2011.07.023
    [Abstract](1554) [HTML](0) [PDF 10.80 M](888)
    Abstract:
    The normal method to determine the trace brominated flame retardants such as polybrominated biphenyls (PBBs) and polybrominated diphenylethers (PBDEs) contained in the electronic and electrical products is gas chromatography/mass spectrometry (GC/MS). However, the method is based on the determinations of the persistent organic pollutants (POPs) such as polychlorinated biphenyls (PCBs), and polychlorinated naphthalene (PCNs) etc. The interferences of those compounds are inevitable. Therefore, in order to overcome this problem, two methods e.g. 1) The combination use of gas chromatography negative ion chemical ionization mass spectrometry (GC-NICI-MS) and gas chromatography-electron impact-mass spectrometry (GC-EI-MS) is employed, 2) a matrix solid-phase dispersion (MSPD) method with YMC ODS-C18 as carrier is developed. The result show that, by the former method, the brominated isomers or ramifications are distinguished remarkably from other halogen compounds because that anion fragment retention peaks of [Br]-, [HBr2]- and molecule chain fragment retention peaks of [M+2]+,[M+4]+,[M+6]+,[M+8]+ are observed simultaneously, and thus the selectivity to determine bromine-containing retardant flames is greatly improved. Using the latter method, the gas chromatographic peaks of multiple polychlorinated biphenyls and polybrominated diphenylethers can be efficiently separated. Thus provides a project to solve interferences of POPs in brominated flame retardants’ determinations. The standard addition experimental results of 10 kinds of BDEs/PCBs belonging to 8 sorts of electronic and electrical equipment show this method has a high precision and reliability due to 60%~98% recovery and <9.5% relative error, which meet the needs regulated by the IEC Commission. It provides a technical support for electronic and eletrical industries in China to further comply with RoHS directive.

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