固相萃取-超高效液相色谱/三重四极杆质谱法同时测定地表水中8种亚硝胺类化合物

建立了固相萃取（SPE）-超高效液相色谱/三重四极杆串联质谱（UPLC-MS/MS）同时测定地表水中8种亚硝胺类化合物的方法。水样中目标物经椰壳活性炭固相萃取小柱吸附富集，小柱经氮气吹干后采用二氯甲烷洗脱。待测样品采用Atlantis T₃柱，以水-甲醇作为流动相进行梯度洗脱，大气压力化学电离源（APCI）正离子模式多反应监测方式（MRM）进行检测，内标法定量分析。8种目标物在相关线性范围内线性良好(r≥0.9950)，地表水加标回收率为55.4%~90.4%，相对标准偏差为3.1%~14.3%，方法检出限为1.1 ~1.8 ng/L。本方法准确度和灵敏度高，适用于快速测定地表水中8种亚硝胺类化合物含量。     

环境检测中地表水检测现状及进展

地表水作为维持人类正常生产生活的重要资源,应作为环境监测的首要任务常抓不懈。现今对地表水的检测工作中仍存在较多不完善之处,应从环境保护的大局出发,应用合理的检测技术,将地表水检测工作提升到新的高度。本文分析了环境检测中地表水的检测现状,并提出了相应的解决措施。     

地表水环境遥感监测关键技术与系统

本文主要是围绕地表水环境遥感检测展开讨论,全面介绍了水环境检测的关键技术和系统,建立改进双峰法的水体分布遥感提取方法,并以具体地区为例进行分析,采用不同方法建立解析方法,从根本上提升反演方法的区域和积极适用性,希望能够对相关人员起到参考性价值。     

氨气敏电极法和纳氏试剂分光光度法对地表水中氨氮的比对测试

采用不同质量浓度的氨氮标准样品和实际样品,用氨气敏电极法和纳氏试剂分光光度法进行同步测试。结果表明,2种分析方法在水样氨氮质量浓度在0. 159～2. 81 mg/L范围内具有良好的可比性、精密性和准确性。氨气敏电极法的检出限为0. 03 mg/L,平行6次测定样品的相对标准偏差为0. 4%～4. 2%,加标回收率为85. 0%～110%;纳氏试剂分光光度法的检出限为0. 025 mg/L,平行6次测定样品的相对标准偏差为0. 5%～6. 4%,加标回收率为93. 0%～99. 8%。同时氨气敏电极法在样品预处理、试剂配制和分析时间上要优于纳氏试剂分光光度法。氨气敏电极法能够满足地表水自动监测在线比对实际工作的需求,该方法具有良好的适用性。     

基于ZIF-L的微固相萃取技术测定地表水中痕量典型多环芳烃

制备类沸石咪唑酯骨架ZIF-L材料,将其用作微固相萃取吸附剂,处理水中萘、苊、苊烯、芴、菲、蒽、荧蒽、芘等8种痕量典型多环芳烃,再用HPLC测定。试验表明,ZIF-L对上述多环芳烃的萃取效率明显高于商品化萃取材料C 18和多壁碳纳米管。方法在0.100μg/L^200μg/L范围内线性良好,方法检出限为0.02μg/L^0.03μg/L,标准溶液5次测定结果的RSD为4.7%~9.5%,实际水样加标回收率为84.5%~115%。将该方法用于北太湖5个点位水样的测定,测定值为未检出~3.40μg/L。     

振荡辐射下PMMA 热解与着火过程研究

采用正弦波变化振荡的辐射热流,对热厚PMMA(聚甲基丙烯酸甲酯)的热解和着火过程进行研究,同时采用数值模拟,对实验结果进行验证和补充。结果表明,表面温度和深度温度随着时间而增加,温度由于周期性的辐射而发生振荡,而振荡幅度随着深度的增加而衰减;表面温度与深度温度振荡存在时间延迟;着火时间随着热流振荡周期的增大而减小,主要由于平均热流密度随着周期增大而增大。     

Catalytic oxidation of CO over Pt/Fe3O4 catalysts: Tuning O2 activation and CO adsorption

• Strong metal-support interaction exists on Pt/Fe₃O₄ catalysts. • Pt metal particles facilitate the formation of oxygen vacancies on Fe₃O₄. • Fe₃O₄ supports enhance the strength of CO adsorption on Pt metal particles. The self-inhibition behavior due to CO poisoning on Pt metal particles strongly impairs the performance of CO oxidation. It is an effective method to use reducible metal oxides for supporting Pt metal particles to avoid self-inhibition and to improve catalytic performance. In this work, we used in situ reductions of chloroplatinic acid on commercial Fe₃O₄ powder to prepare heterogeneous-structured Pt/Fe₃O₄ catalysts in the solution of ethylene glycol. The heterogeneous Pt/Fe₃O₄ catalysts achieved a better catalytic performance of CO oxidation compared with the Fe₃O₄ powder. The temperatures of 50% and 90% CO conversion were achieved above 260°C and 290°C at Pt/Fe₃O₄, respectively. However, they are accomplished on Fe₃O₄ at temperatures higher than 310°C. XRD, XPS, and H₂-TPR results confirmed that the metallic Pt atoms have a strong synergistic interaction with the Fe₃O₄ supports. TGA results and transient DRIFTS results proved that the Pt metal particles facilitate the release of lattice oxygen and the formation of oxygen vacancies on Fe₃O₄. The combined results of O₂-TPD and DRIFTS indicated that the activation step of oxygen molecules at surface oxygen vacancies could potentially be the rate-determining step of the catalytic CO oxidation at Pt/Fe₃O₄ catalysts. The reaction pathway involves a Pt-assisted Mars-van Krevelen (MvK) mechanism.     

舟山高浊度海水混凝除浊研究

测定了舟山高浊度海水悬浮物的粒度分布,分析了高浊度海水自由沉降特性,选用氯化铁(FeCl)3、聚合氯化铁(PFC)、聚合硫酸铁(PFS)3种混凝剂,利用正交试验方法对高浊度海水进行混凝沉淀对比试验,采用极差分析方法研究了影响混凝效果的因素。试验结果表明:舟山海域悬浮物组成以粉砂为主,用自然沉降的方法是很难去除;各因素对浊度去除率影响的主次顺序均为:慢搅时间>慢搅速度>快搅时间>快搅速度;对于高浊度海水混凝除浊最佳水力条件为:快搅时间为2 min,快搅速度为300 r/min,慢搅时间为15 min,慢搅速度为60 r/min;聚合硫酸铁是较理想的絮凝剂,最佳投药量范围在15～25 mg/L,对浊度去除率高达99%以上。     

Entry and toxicity of organic pesticides and copper in vineyard streams: Erosion rills jeopardise the efficiency of riparian buffer strips

The present study was performed to characterise in-stream pesticide exposure within the Palatinate vineyard region in south-west Germany, evaluate the influence of buffer strip widths and identify mitigation measures for the relevant entry pathways. In-stream water and sediment samples that were taken at nine sampling sites of different buffer widths following intense rainfall, and edge-of-field runoff that were sampled in erosion rills were analysed regarding 28 active ingredients of pesticides including copper. In-stream samples contained a mix of 8 ± 4 pesticide compounds, resulting in total pesticide concentrations of 1.4-8.9 μg l⁻¹ for water and 16-670 μg kg⁻¹ dw for sediment. Following an exceptional rainfall event with a previous 34-day drought period, pesticide concentrations reached 7.0-83.4 μg l⁻¹. Fungicides were the most important pesticides found and were significantly correlated with the pesticide application frequency and rate. The calculated toxicity values per sample (TU_max) indicated that both organic pesticides and copper concentrations likely cause ecotoxicological effects in the field. The buffer strip width was of little importance for pesticide in-stream concentrations because pesticide entry occurred mainly via the field path network and erosion rills. Pesticide in-stream concentrations were significantly and positively correlated with the concentrations detected in erosion rills (R² = 0.56). As possible risk mitigation measures, we suggest the implementation of grassed field paths and vegetated ditches or wetlands.     

水体系中氧氟沙星的光化学降解研究

研究了高压汞灯和氙灯照射下氧氟沙星(OFLX)在蒸馏水、人工海水和天然海水中的光降解过程,探讨了光源、起始浓度、丙酮、表面活性剂等因素对OFLX光化学降解速率的影响.结果表明,OFLX在高压汞灯下的光反应速率比在氙灯下快得多,均符合一级反应动力学过程;在相同光源下,OFLX在海水中降解最快,其次是人工海水;当OFLX初始浓度为2、4、6mg.L-1时,其光解速率常数分别为0.163、0.140和0.132 min-1,随着OFLX初始浓度增大,其光解率降低;不同浓度的丙酮均能促进OFLX光降解的反应,其反应速率常数为0.084 2～0.102 min-1,且光敏效率与丙酮浓度呈正相关关系;然而当十六烷基三甲基溴化铵(CTAB)、十二烷基苯磺酸钠(SDBS)、吐温-20(TW-20)等表面活性剂的浓度为5 mg.L-1,它们均抑制了水体中OFLX光降解反应的进程.另外,利用金藻8701单种培养进行了OFLX光化学降解前后的毒性试验,表明OFLX光解过程产生风险较高的中间产物,随着光解进行,产物毒性降低.