氟虫双酰胺在水稻和稻田中的残留动态研究

采用超高效液相色谱法(UPLC)测定了氟虫双酰胺19.8%悬浮剂(SC)在水稻及稻田环境中的残留动态.结果表明,当氟虫双酰胺及其代谢产物NNI-des-iodo的添加量为0.05～1.0 mg·kg-1时,其在水稻田土壤、田水、稻秆、稻米和稻壳中的平均回收率为78.2%～104.8%,变异系数为1.1%～4.4%.氟虫双酰胺在2011年三地(福建福州、天津、江苏南京)的稻田水中的降解半衰期为9.8～17.3 d,土壤中10.8～22.4 d,植株中7.6～17.3 d,其在稻田水样品中检出了代谢产物NNI-des-iodo,而在土壤和植株样品中未检出.在推荐使用剂量下,于末次施药10 d后,氟虫双酰胺在水稻稻米中的残留量均低于美国规定的在稻谷上的最大残留允许量(0.5 mg·kg-1).     

单光子/光电子在线质谱实时分析聚氯乙烯热分解/燃烧产物

实验室研制了低能光电子磁场增强电离(MEPEI)和单光子电离(SPI)复合电离源,该电离源具有电离化合物范围宽、碎片离子少、质谱图简单等优点,结合飞行时间质谱(TOF-MS)实现了聚氯乙烯(PVC)热分解/燃烧产物的在线分析.针对不同的目标化合物,MEPEI/SPI复合电离源通过调节电离区电场强度,可以快速在SPI和SPI-MEPEI之间切换.PVC热分解/燃烧产物中电离能大于光子能量(10.60 eV)的HCl和CO2(12.74 eV、13.77 eV)利用MEPEI模式电离;而烯烃、二氯乙烯、苯系物、氯苯、苯乙烯、茚满及萘系物等可通过SPI-MEPEI复合模式电离.通过实时监测PVC主要燃烧产物的信号强度随温度的变化趋势可推断出,PVC燃烧产物主要是通过两种机制生成:①250～370℃时,PVC发生脱氯及分子内环化反应,产生大量的HCl、苯和萘;②380～510℃时,PVC发生分子间交联反应,生成烷基芳烃,如甲苯和二甲苯/乙苯等.实验结果表明,SPI/SPI-MEPEI复合离子源TOF-MS分析速度快,应用范围广,在在线分析中具有广泛的应用前景.     

Application of comprehensive two-dimensional gas chromatography with mass spectrometric detection for the analysis of selected drug residues in wastewater and surface water

Pharmaceutical residues have become tightly controlled environmental contaminants in recent years, due to their increasing concentration in environmental components. This is mainly caused by their high level of production and everyday consumption. Therefore there is a need to apply new and sufficiently sensitive analytical methods, which can detect the presence of these contaminants even in very low concentrations. This study is focused on the application of a reliable analytical method for the analysis of 10 selected drug residues, mainly from the group of non-steroidal anti-inflammatory drugs (salicylic acid, acetylsalicylic acid, clofibric acid, ibuprofen, acetaminophen, caffeine, naproxen, mefenamic acid, ketoprofen, and dicofenac), in wastewaters and surface waters. This analytical method is based on solid phase extraction, derivatization by N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) and finally analysis by comprehensive two-dimensional gas chromatography with Time-of-Flight mass spectrometric detection (GC×GC- TOF MS). Detection limits ranged from 0.18 to 5 ng/L depending on the compound and selected matrix. The method was successfully applied for detection of the presence of selected pharmaceuticals in the Svratka River and in wastewater from the wastewater treatment plant in Brno-Modrice, Czech Republic. The concentration of pharmaceuticals varied from one to several hundreds of ng/L in surface water and from one to several tens of μg/L in wastewater.     

Preparation of MgO/B2O3 coatings by plasma spraying on SUS304 surface and effects of heat-resistant

This study mainly deals with the preparation of MgO/B₂O₃ coatings by plasma spraying on the SUS304 surface and the effects of heatresistant. The power materials of low thermal conductivity were selected to control the heat divergent performance of high temperature parts. The reticular micro-structure between the cover thermal layer and the substrate was prepared by using the plasma spraying method. The powder mixture of MgO and B₂O₃ were selected as spraying materials and the SUS304 was used as the substrate material. The MgO/B₂O₃ coating was prepared on the surface of the SUS304 to provide better cover thermal performance. The properties of the microstructures and the morphologies were studied by Optical Microscope, Scanning Electron Microscope, Electron Probe Microanalyzer, and X-ray Diffraction. The results showed that the cover thermal performance has been improved.     

Simultaneous preconcentration of cadmium and lead in water samples with silica gel and determination by flame atomic absorption spectrometry

A new method that utilizes pretreated silica gel as an adsorbent has been developed for simultaneous preconcentration of trace Cd(II) and Pb(II) prior to the measurement by flame atomic absorption spectrometry. The effects of pH, the shaking time, the elution condition and the coexisting ions on the separation/preconcentration conditions of analytes were investigated. Under optimized conditions, the static adsorption capacity of Cd(II) and Pb(II) were 45.5 and 27.1mg/g, the relative standard deviations were 3.2% and 1.7% (for n = 11), and the limits of detection obtained were 4.25 and 0.60 ng/mL, respectively. The method was validated by analyzing the certified reference materials GBW 07304a (stream sediment) and successfully applied to the analysis of various treated wastewater samples with satisfactory results.     

Homogeneous and heterogeneous reactions of anthracene with selected atmospheric oxidants

The reactions of gas-phase anthracene and suspended anthracene particles with O3 and O3-NO were conducted in a 200-L reaction chamber, respectively. The secondary organic aerosol (SOA) formations from gas-phase reactions of anthracene with O3 and O3-NO were observed. Meanwhile, the size distributions and mass concentrations of SOA were monitored with a scanning mobility particle sizer (SMPS) during the formation processes. The rapid exponential growths of SOA reveal that the atmospheric lifetimes of gas-phase anthracene towards O3 and O3-NO are less than 20.5 and 4.34 hr, respectively. The particulate oxidation products from homogeneous and heterogeneous reactions were analyzed with a vacuum ultraviolet photoionization aerosol time-of-flight mass spectrometer (VUV-ATOFMS). Gas chromatograph/mass spectrometer (GC/MS) analyses of oxidation products of anthracene were carried out for assigning the time-of-flight (TOF) mass spectra of products from homogeneous and heterogeneous reactions. Anthrone, anthraquinone, 9,10- dihydroxyanthracene, and 1,9,10-trihydroxyanthracene were the ozonation products of anthracene, while anthrone, anthraquinone, 9-nitroanthracene, and 1,8-dihydroxyanthraquinone were the main products of anthracene with O3-NO.     

LNAPLs污染物在层状非均质多孔介质中的运移试验研究

文章通过室内试验研究层状非均质多孔介质中轻非水相液体(Light Non-Aqueous Phase Liquid,LNAPL)的运移机制与分布特性。首先,在二维砂槽上进行LNAPL的入渗试验,试验过程中用数码相机进行拍照,把LANPL的扩散过程以图像的形式记录下来;然后,用AutoCAD对图片进行分析处理,得出不同时刻LNAPL的入渗锋面变化图。结果发现,介质结构突变面改变了LNAPL的迁移模式。在LNAPL由中砂进入细砂层后,由于受到毛细作用的增强,其运移速度加快;而由中砂进入粗砂,受粗砂介质阻滞作用增强的影响,LNAPL运移速度变小。当LNAPL由干砂进入湿润砂体时,由于孔隙水浮托力增大,LNAPL先产生纵向运移,随后以横向迁移的形式在地下水位上部聚积。当达到一定厚度后,LNAPL的压头足以克服浮托力,驱替孔隙水进入砂土孔隙。另外,LNAPL的厚度足够大时,方可克服饱水层受到的浮托力,在地下水位上形成LNAPL池,并因孔隙水向周围砂体排泄,LNAPL池周围的水位上升。     

基于单颗粒质谱信息气溶胶分类方法的研究进展

气溶胶质谱仪在对气溶胶颗粒的监测过程中会产生大量单颗粒的化学成分和粒径信息,基于这些质谱数据能够推测颗粒的来源。而对气溶胶来源的分析,很大程度上是由颗粒的种类决定的,故对海量数据的分类就成为不可忽略的步骤。针对气溶胶质谱仪采集到的数据,概述了用于气溶胶分类的多种方法的理论核心、分类步骤及各自的优缺点等。据此可为今后气溶胶分类方法的研究提供建设性意见。     

离子色谱法测定环境空气中丁酸

建立了用离子色谱法测定环境空气中丁酸的新方法。对实际样品进行分析,丁酸的回收率为94．5％-103．8％,当采样体积为60L时环境空气中丁酸的检出限为0．003mg／m^3。本方法分析速度快,所需样品量少,且无需复杂的前处理,简便、灵敏、可靠。     

气相色谱法测定大气中乙酸乙酯和甲基丙烯酸甲酯

建立了用气相色谱法测定大气中乙酸乙酯和甲基丙烯酸甲酯的方法。大气中乙酸乙酯和甲基丙烯酸甲酯活性炭吸附,二硫化碳解吸,DB-200毛细管柱分离,直接进样分析,氢火焰离子化检测器检测,时间定性,峰面积定量。本方法前处理简便,分离度好,分析灵敏度高,满足环境分析要求。