高效液相色谱法测定地下水中洛克沙胂

地下水水样经磷酸二氢钾提取后,用MAX固相萃取小柱对其净化、浓缩,再用高效液相色谱仪测定样品中的洛克沙胂。对色谱条件进行优化,使该方法在0.500 mg/L~10.0 mg/L范围内线性良好,方法检出限为0.047μg/L。空白加标样6次测定结果的RSD为5.3%,空白水样的3个质量浓度水平的加标回收率为79.8%~88.8%。将该方法用于测定6个地下水实际样品中洛克沙胂,其中1个被检出,测定值为0.42μg/L。     

气相色谱/质谱法测定水中15种酞酸酯类化合物

采用固相萃取-气相色谱/质谱法测定水中15种酞酸酯类化合物,确定方法的最优条件为:依次用10 m L正己烷和丙酮混合溶剂(V/V=5∶1)、甲醇和空白试剂水活化C18固相萃取柱后,水样以5 m L/min过柱萃取,再以8 m L正己烷:丙酮(V/V=5∶1)混合溶剂洗脱后,浓缩至1 m L,进气相色谱/质谱测定。该法的检出限为0.18~0.38μg/L,在0.50~20.0 mg/L范围内线性良好,相关系数均0.996。空白水样的加标回收率为71.8%~120%,相对标准偏差为1.73%~12.7%;实际废水水样的加标回收率为64.8%~135%,相对标准偏差为2.75%~18.0%。     

堤防工程综合安全模型和风险评价体系研究及应用

为获得荆南长江干堤的安全特性,在层次分析法及模糊一致理论的基础上,考虑堤防工程水、土两相系材料的特点,建立了模糊综合评判系统结构模型。通过正态型模糊隶属函数,结合两种权值理论实现了对堤防工程的安全综合评判。在模糊综合评判结论的基础上,结合模式识别的间接方法,提出了广义多维加权模糊识别模型,实现了对典型堤身段的安全模式识别,并对模型指标体系作了敏感性分析。所得成果比较全面地反映了干堤在复杂运行条件下的综合安全特性,对指导工程现场管理与监测有现实意义。对于复杂堤防系统,模糊综合评判是实现全面风险分析的有效手段,而广义多维加权模糊识别模型可以为工程安全决策提供有力依据。     

Microwave/SPME method to quantify pesticide residues in tomato fruits

A new analytical method using focused microwave-assisted extraction (FMAE), coupled with solid phase micro-extraction (SPME), has been elaborated to determine 25 pesticides used in tomato cultivation. Microwave energy was used for a fast and controlled heating of solvent to selectively extract compounds. Calibration curves were plotted from blank tomato samples spiked at different concentrations with standards. A linear response was obtained between 10 and 1000 μ g/Kg for pyrethroids and between 0.1 and 5000 μ g/Kg for other compounds. For all studied substances, the resulting correlation coefficient (r²) was greater than 0.99. Limits of detection (LOD) and quantification (LOQ) were measured lower than 8 and 25 μ g/Kg, respectively. The relative standard deviation (RSD) was determined below 15% for all pesticides. Field incurred tomato samples were used to validate the new FMAE/SPME method. Observed analysis results by using this technique were in good agreement compared to those obtained by two accredited trading laboratories using traditional methods. Four tomato samples, bought in a local market, were also tested with the FMAE/SPME method.     

利用某尾矿制备纳米SiO2

采用固相熔融法从尾矿中提取SiO2,利用超声辅助化学沉淀法制备纳米SiO2。分别研究了NaOH与尾矿质量比、反应温度、反应时间对SiO2提取率的影响,以及溶解水量、HCl浓度、终点pH、超声波功率和超声波频率对纳米SiO2性能的影响,研究表明,当NaOH与尾矿的质量比为1.4∶1,温度为325℃时灼烧25 min后用100 mL水溶解,滴加1.6 mol/LHCl酸化沉淀,终点pH调至8.5,在超声功率100 W,超声频率28 Hz的条件下,尾矿中SiO2提取率达到98.0%,产物中SiO2含量为98.40%,平均粒度为18 nm,得到的产品符合国家标准。     

气液两相旋流喷嘴雾化特性

为提高烟尘净化用喷嘴的雾化性能,提出一种气液两相旋流喷嘴,用CFX软件对该喷嘴内部流场模拟的结果表明,强烈的气旋作用使液流呈环状,使气液混合流在达到喷嘴末端时易于破碎成雾。在实验室条件下,利用Winner313型喷雾激光粒度分析仪对喷嘴进行了雾化粒度测定,分析发现雾滴中位径与气液比的关系呈幂函数衰减,这一规律将有助于在工程应用时确定喷嘴工况。     

Interaction of bisphenol A with dissolved organic matter in extractive and adsorptive removal processes

The fate of endocrine disrupting chemicals (EDCs) in natural and engineered systems is complicated due to their interactions with various water constituents. This study investigated the interaction of bisphenol A (BPA) with dissolved organic matter (DOM) and colloids present in surface water and secondary effluent as well as its adsorptive removal by powdered activated carbons. The solid phase micro-extraction (SPME) method followed by thermal desorption and gas chromatography-mass spectrometry (GC-MS) was utilized for determining the distribution of BPA molecules in water. The BPA removal by SPME decreased with the increased DOM content, where the formation of BPA-DOM complexes in an aqueous matrix was responsible for the reduced extraction of BPA. Colloidal particles in water samples sorbed BPA leading to the marked reduction of liquid phase BPA. BPA-DOM complexes had a negative impact on the adsorptive removal of BPA by powered activated carbons. The complex formation was characterized based on Fourier transform infrared (FTIR) and ultraviolet-visible (UV-Vis) spectroscopy, along with the calculation of molecular interactions between BPA and functional groups in DOM. It was found that the hydrogen bonding between DOM and BPA would be preferred over aromatic interactions. A pseudo-equilibrium molecular coordination model for the complexation between a BPA molecule and a hydroxyl group of the DOM was developed, which enabled estimation of the maximum sorption site and complex formation constant as well as prediction of organic complexes at various DOM levels.     

我国生活垃圾焚烧工程分析

分析了我国生活垃圾的基本特征、垃圾焚烧厂的效益和垃圾焚烧厂的现状,展望了我国垃圾焚烧工程的发展趋势。     

Validation and use of in vivo solid phase micro-extraction (SPME) for the detection of emerging contaminants in fish

A variety of emerging chemicals of concern are released continuously to surface water through the municipal wastewater effluent discharges. The ability to rapidly determine bioaccumulation of these contaminants in exposed fish without sacrificing the animal (i.e. in vivo) would be of significant advantage to facilitate research, assessment and monitoring of their risk to the environment. In this study, an in vivo solid phase micro-extraction (SPME) approach was developed and applied to the measurement of a variety of emerging contaminants (carbamazepine, naproxen, diclofenac, gemfibrozil, bisphenol A, fluoxetine, ibuprofen and atrazine) in fish. Our results indicated in vivo SPME was a potential alternative extraction technique for quantitative determination of contaminants in lab exposures and as well after exposure to two municipal wastewater effluents (MWWE), with a major advantage over conventional techniques due to its ability to non-lethally sample tissues of living organisms.