苦味酸测定中关键问题的研究

目前测定苦味酸的国标方法为《生活饮用水标准检验方法有机物指标》(GB/T 5750.8—2006)中的衍生物-液液萃取-气相色谱法,在实际测试过程中,发现水样pH值和基质效应会影响苦味酸测定。当pH值为8~12时,生成的氯化苦响应强度变化不大;在pH约为13时,响应强度最大。水质中除腐殖酸、硝基甲烷及2,4,6-三硝基甲苯会影响苦味酸测定外,硝基酚类和甲基酚类同样起到正干扰作用,因此,国标方法不能全面和准确地测定水中的苦味酸含量。     

Morphological characteristics of flashing jet throughout superheated liquid release

Many release problems involve two-phase releases of hazardous materials of superheated liquids with high energy into the atmosphere. Such accidents are accompanied by violent phase transition and form catastrophic flashing jets. In this work, experimental and theoretical analyses were conducted to investigate dynamic characteristics of flashing jet morphology and their dependence on pressure-decay dynamics under different storage pressures, superheats, and nozzle diameters. Flashing jet morphology and angle throughout two-phase releases were captured by a high-speed camera, and the corresponding source pressure in the superheated liquid tank was measured simultaneously. Results show that three typical phases, expansion, stabilization, and decay, are characterized throughout two-phase release based on the evolution of flashing jet morphology. The jet initially expands gradually due to the enhancement of phase transition intensity, and then keeps stable when the intensity reaches its maximum, and terminally decays rapidly due to the depletion of superheated liquid. Phase transition intensity at the nozzle exit is mainly controlled by the pressure-decay dynamics. Bubbles nucleation inception sites gradually move upstream of the nozzle during the pressure decay process increasing the phase transition intensity. The increase of storage pressure, superheat and nozzle diameter promotes the mechanical and thermodynamic effects on the jet breakup. The significant increase of mechanical and thermodynamic effects effectively accelerates droplets evaporation and further affects flashing jet morphology.     

Experimental investigation of the lower flammability limit of volatile liquid fuel-aluminum powder mixtures in air

Aluminum powder was always chosen as an additive to improve the explosive performance. In this work, experiments were performed to investigate the lower flammability limit (LFL) of volatile liquid fuel-aluminum powder mixtures using a 20 L closed spherical stainless steel vessel at a temperature of 20 °C (293 K) and 40 °C (313 K). The volatile liquid fuels tested in the work were diethyl ether (DEE), epoxypropane (PO), n-pentane and n-hexane. DEE, PO and n-pentane are in the liquid phase at room temperature and can easily transition to the gas phase at 40 °C (313 K). Through a series of experiments carried out, it was found that the change in phase would affect the interaction between the components. Aluminum powder always has an inhibitory effect on the flammability of the mixtures when it is mixed with gas-phase fuels. The inhibition effect was most obvious when the aluminum powder concentration reached 200 g/m³. While the interaction between aluminum powder and liquid-phase volatile fuels was promotion and was influenced by the component proportion and the type of the volatile fuels.     

Dissipation of Endosulfan and Dichlorvos Residues In/On Cauliflower Curds

Dissipation behaviour of endosulfan and dichlorvos in/on cauliflower, variety Snowball-16, was studied during rabi season (Sep.–March) 2003–2004. Endosulfan and dichlorvos were sprayed @ 350 and 110g a.i. with 115 g a.i., respectively, 80 days after transplanting. Samples were taken at the interval of 0 (1h after spray), 3, 5, 7, and 10 days after spray (DAS) in triplicate and residues were estimated on GC-ECD system equipped with capillary column. The initial deposits of 3.452 and 0.295μgg⁻¹ of endosulfan and dichlorvos dissipated to 0.084 (97.56%) and 0.009 (96.95%), respectively after 10 DAS. Residues of endosulfan reached below maximum residue limit of 2μgg⁻¹ one day after spray and of dichlorvos were below MRL value of 0.5μgg⁻¹ even on 0 day. Dissipation pattern followed first order kinetics for both the insecticides with half life periods of 1.81 and 2.08 days for endosulfan and dichlorvos, respectively.     

超高效液相色谱法测定土壤中微量阿特拉津

采用超高效液相色谱仪,建立了土壤中微量阿特拉津的快速检测方法.研究结果表明:采用反相C18色谱柱,以甲醇/水(70:30,v/v)为流动相,流速为0.2 ml/min,柱温为30℃,检测波长为220 nm条件下,在12.5～1000μg/L质量浓度范围内线性关系良好(r=0.9999),检出限0.18×10-3 mg/...     

基于ACF-AMDF的气井环空液面回波特征提取方法

为了精确有效地提取声波法检测气井环空液位的回波周期,在分析环空中测试波的传播特征及基音周期检测的基础上,提出1种基于检测信号短时自相关函数(ACF)及平均幅度差函数(AMDF)的液面回波周期提取方法;利用自主搭建的室内模拟实验系统开展了不同初始环空压力下环空液位检测实验;对检测信号进行中心削波处理并计算ACF/AMDF,提取出液面回波周期并与理论计算值对比分析;同时分析了现场环空液位检测信号,提取其回波周期。研究结果表明:提出的新方法能有效地用于提取环空液面回波周期;室内实验中,该方法最大误差绝对值为1.54%;该方法能够有效抑制液面回波信号中的随机噪声及接箍反射波等,处理后的信号曲线在回波周期处峰值更加突出、集中,而在其他位置更加平滑,提高了对液面回波周期特征的辨识能力。     

生物滴滤塔处理氯苯废气的工艺性能

将活性污泥培养及驯化后接种于生物滴滤塔中,挂膜启动后处理模拟氯苯废气（简称氯苯废气）,考察了生物滴滤塔在挂膜启动阶段及稳定运行阶段的性能。实验结果表明：接种41 d后生物滴滤塔成功挂膜,此时氯苯去除率稳定在90%以上;生物滴滤塔稳定运行阶段,随着进气中氯苯质量浓度由303.82 mg/m³逐渐增至1 489.05 mg/m³,氯苯去除率从85.1%降至70.1%。处理氯苯废气适宜的工艺条件为：空塔停留时间超过45 s,喷淋液流量31.8 mL/min,氯苯负荷23.97~128.01 g/（m³·h）。生物滴滤塔对喷淋液的酸性环境有较好的适应性,喷淋液pH的变化对氯苯去除率无显著影响。     

Decay profile and metabolic pathways of quinalphos in water, soil and plants

The widespread occurrence of pesticide residues in different agricultural and food commodities has raised concern among the environmentalists and food chemists. In order to keep a proper track of these materials, studies on their decay profiles in the various segments of ecosystem under varying environmental conditions are needed. In view of this, the metabolites of quinalphos in water and soil under controlled conditions and in plants, namely tomato and radish in field conditions have been analysed and possible pathways suggested. In order to follow the decay of the pesticide, an HPLC procedure has been developed. Studies conducted in water at different temperatures, pH and organic content reveal that the persistence of the pesticide decreases with the increase in all the three variables. In the three different types of soils studied, the effect of pH is more or less apparent on a similar line. On an average a faster decay is observed in the case of plants than in water and soil. The decay profiles in all these cases follow first order kinetics. The metabolites were identified by GC-MS. The investigations reflect that degradation occurs through hydrolysis, S-oxidation, dealkylation and thiono-thiol rearrangement. The pathways seem to be complex and different metabolites were observed with the change in the matrix. Quinalphos oxon, O-ethyl-O-quinoxalin-2-yl phosphoric acid, 2-hydroxy quinoxaline and quinoxaline-2-thiol were observed in all the matrices. Results further indicate that the metabolites, 2-hydroxy quinoxaline and oxon, which are more toxic than parent compound, persist for a longer time.     

Pressurized liquid extraction of six tetracyclines from agricultural soils

Veterinary antibiotics used in agriculture can be introduced into the environment through land application of animal manure, accumulating in soils and groundwaters and posing a significant risk to human health and animal well-being. As the analysis of tetracyclines in soil is challenging due to their strong interaction with soil minerals and organic carbon, the objective of this study was to develop a reliable and reproducible method for quantitative analysis of chlortetracycline and oxytetracycline, and their respective metabolites in soils. A method based on pressurized liquid extraction (PLE) with in-cell clean-up was developed for the extraction of chlortetracycline and oxytetracycline and four likely metabolites from a set of four soils. Optimized conditions included a cell size of 22?mL, soil loading of 5?g, pH of 8.0, methanol:water ratio of 3:1, 50?°C, and two cycles. Soil extracts were analysed by high-performance liquid chromatography (HPLC) coupled with ion trap mass spectrometry (MS). Recoveries of seven tetracyclines from soil ranged from 41% to 110%. The limits of detection for tetracyclines were 0.08–0.3 µg g^?1 soil, and intra- and inter-day variation ranged from 0.12–0.34%. The proposed PLE method is suitable for quantification of tetracyclines in agricultural soils at typical concentrations expected in contaminated environments.     

Investigation of titanium liquid/gas diffusion layers in proton exchange membrane electrolyzer cells

In a proton exchange membrane electrolyzer cell (PEMEC), liquid/gas diffusion layer (LGDL) is expected to transport electrons, heat, and reactants/products to and from the catalyst layer with minimum voltage, current, thermal, interfacial, and fluidic losses. In addition, carbon materials, which are typically used in PEM fuel cells (PEMFCs), are unsuitable in PEMECs due to the high ohmic potential and highly oxidative environment of the oxygen electrode. In this study, a set of titanium gas diffusion layers with different thicknesses and porosities are designed and examined coupled with the development of a robust titanium bipolar plate. It has been found that the performance of electrolyzer improves along with a decrease in thickness or porosity of the anode LGDL of titanium woven meshes. The ohmic resistance of anode LGDL and contact resistance between anode LGDL and the anode catalyst play dominant roles in electrolyzer performance, and better performance can be obtained by reducing ohmic resistance. Thin titanium LGDLs with straight-through pores and optimal pore morphologies are recommended for the future developments of low-cost LGDLs with minimum ohmic/transport losses.