Rapid determination of polar pesticides and plant growth regulators in fruits and vegetables by liquid chromatography/tandem mass spectrometry

ABSTRACT

A simple high-throughput liquid chromatography/tandem mass spectrometry (LC-MS/MS) multiresidue analysis method was developed for the simultaneous determination of polar pesticides, plant growth regulators and other polar compounds. These included amitrole, chlormequat, mepiquat, cyromazine, ETU, PTU, perchlorate, and daminozide using a mixed-mode column. A 10 g test portion was shaken with acidified methanol for 10 min. After centrifugation, the sample extract was injected and analyzed within 11 min by LC-MS-MS. This column eliminated the need for derivatization or the use of ion paring reagent. Two MS-MS transitions were monitored in the method for each target compound to achieve true positive identification. Eight isotopically-labeled internal standards corresponding to each analyte were used to correct for matrix suppression effect and/or instrument signal drift. The average recovery for all analytes at 20, 40, and 250 ng/g (n = 6) ranged from 73–136%, with a relative standard deviation of ≤ 20%.     

叠式空气隙膜蒸馏组件膜污染实验研究

采用一种具有旋流结构的多层层叠式空气隙膜蒸馏膜组件,以20 g/L氯化钠盐水为热工质,考察在70℃条件下膜污染情况,实验结果表明,一个周期的连续运行和间歇性操作膜表面在高温下较快进入膜污染,8个周期后膜通量下降为初始通量的42%。膜表面有大量黄色附着物,电镜SEM分析显示,膜表面被不均匀堆积的颗粒状污染物及长方体结晶物覆盖,能谱EDS分析,污染物有极少量NaCl结晶的Na、Cl元素,还有O、C、Mg、Cu和Fe等元素。污染膜经5%盐酸溶液清洗后无机垢沉淀被去除,表观效果较好。     

密相半干法低温同时脱硫脱硝影响因素

针对90~160℃的低温条件下,SO₂对钙基吸收剂吸收NO_x的影响进行了实验研究,分析了烟气温度T、含氧率、含湿量等对SO₂促进钙基吸收剂吸收NO_x的影响。实验结果表明,当烟气中SO₂浓度的升高可促进钙基吸收剂对NO_x的吸收;同时,维持反应系统在9.2%的含湿量;保证烟气温度在结露点以上,使系统在90~100℃的温度区间;控制系统漏风率,防止含氧率的升高;保证前端电除尘效率的同时,将一部分电除尘捕集到的灰尘作为钙基脱硫剂的添加剂,并使之参与脱硫反应器内的钙基吸收剂循环过程中;可较多地脱除烟气中的污染物质。     

臭氧微气泡深度处理染料废水生化出水

采用臭氧氧化法对某厂染料废水生化出水进行深度处理,考察了废水初始pH值和臭氧气泡大小对废水处理效果的影响,研究了臭氧微气泡对气液传质的影响。结果表明,在pH 2.5~11范围内,废水初始pH值越大,处理效果越好;加载微孔膜片后,臭氧气泡粒径变小,增大了臭氧的传质比表面积,延长了臭氧气泡在反应柱内的停留时间,强化了传质效果,处理废水的臭氧利用率可增大10%~30%,强化了臭氧氧化作用。加载5 μm孔径的膜片相比无膜片的情况,COD去除率提高了近30%,TOC去除率提高了16%。     

侧沟式一体化OCO工艺中DO和C/N对同步硝化反硝化的影响

以自配模拟生活污水为处理对象,研究了不同DO和C/N对侧沟式一体化OCO反应器同步硝化反硝化和COD降解效果的影响。实验结果表明,维持进水COD均值约为300 mg/L,TN约为40 mg/L,MLSS约为2 600 mg/L,进水流量为20 L/h时,COD去除率随着DO的增大逐步提高,当好氧区DO均值约为2.0 mg/L时,同步硝化反硝化效果最好,TN去除率达到了80%以上;维持好氧区DO均值约为2.0 mg/L,MLSS约为2 600 mg/L,进水流量为20 L/h时,不同C/N对COD去除率影响不大,当进水C/N约为8时,同时硝化反硝化效果最好,TN去除率均值达到了82%。     

分散填料曝气塔多相流态分析与传氧性能表征

针对分散填料曝气塔中多相流的流态与传氧过程,实验了布气方式以及海绵和陶粒2种填料对于体系的气含率εg、流态以及气-液传质性能的影响。在表观气速U范围(0.01～0.18 m/s)内观察到81孔布气板(Φ1 mm)体系出现3个明显相区,孔数过少(25孔),或者孔间距较小(225孔)均没有明显过渡区,在湍流区(U>0.118 m/s)3种布气板的气含率没有明显差别。海绵填料体积分数εs<25%时体系的气含率没有明显变化,35%时气含率下降且过渡区提前出现。在非均相区,海绵填料明显提高了体系的传质系数KLa。陶粒填料降低了气含率,固含率对εg的影响差别不明显,同时降低了多相流体系的KLa,且随着固含率的增加KLa降低。对比多种操作条件,单位体积空气传氧能力KLa/εg无明显差别,但在81孔布气板的过渡区KLa/εg出现一个明显的极小区间,说明过渡区传氧效率较低。在特定的实验操作条件下,KLa/εg较为稳定,这为深入理解两种气泡群体的共存体系在传氧性能方面各自的权重,提供了重要的量化参考。     

气氛含氧量对DDT热处理特性的影响

滴滴涕属于有机氯农药,其所含成分DDTs在环境中难以降解,并具有生物毒性。利用高温管式炉研究气氛中含氧量对滴滴涕热处理特性的影响,为研发废弃滴滴涕高温热处理技术提供理论依据。实验结果表明,在600℃时,滴滴涕去除率最高为含氧量21%时的70.48%;在900℃条件下,当含氧量为21%时DDT去除率≥99%;在1 200℃条件下,当含氧量≥12%时DDT去除率≥99.9%。在滴滴涕热处理残渣中,o,p’-DDT占DDTs总量的比例在3个温度段中都随含氧量的增加而增长,DDT则都随含氧量增加而减少,且上述变化随温度升高而幅度加大。在尾气中,p,p’-DDE占DDTs总量的比例在3个温度段中都随含氧量增加而递增,在1 200℃条件下尤为明显。     

Pilot scale application of a method for the analysis of perfluorinated compounds in surface soils

A growing number of studies now indicate that perfluorinated compounds (PFCs) are globally distributed in the environment. Their widespread distribution and presence in remote locations has led to questions about the importance of atmospheric and oceanic transport. Describing their distribution in surface soils is also an essential but neglected element in developing a comprehensive understanding of their occurrence in the environment. Soils are the critical link between global atmospheric and hydrologic processes where both local and distant contaminants can accumulate and be released into aquatic and terrestrial communities. Because PFC concentrations in soils will influence ground and surface water, wildlife, and crops, methods to accurately measure PFCs in soil are clearly needed. To help answer this need, we developed a method for the analysis of nine perfluorinated carboxylic acids and four perfluorinated sulfonic acids in soil. Samples from six nations (n = 10 per nation) were analyzed by LC-MS/MS to demonstrate the method performance parameters and to make preliminary observations about the occurrence of the PFCs in soils in different parts of the world. The resulting method shows acceptable performance characteristics for the target compounds in most soils while documenting the widespread occurrence of PFCs in surface soils.     

High-molecular weight sulfur-containing aromatics refractory to weathering as determined by Fourier transform ion cyclotron resonance mass spectrometry

Biomarkers and low-molecular weight polyaromatic compounds have been extensively studied for their fate in the environment. They are used for oil spill source identification and monitoring of weathering and degradation processes. However, in some cases, the absence or presence of very low concentration of such components restricts the access of information to spill source. Here we followed the resistance of high-molecular weight sulfur-containing aromatics to the simulated weathering condition of North Sea crude oil by ultra high-resolution Fourier transform ion cyclotron resonance mass spectrometry. The sulfur aromatics in North Sea crude having double bond equivalents (DBE) from 6 to 14 with a mass range 188-674 Da were less influenced even after 6 months artificial weathering. Moreover, the ratio of dibenzothiophenes (DBE 9)/naphthenodibenzothiophenes (DBE 10) was 1.30 and 1.36 in crude oil and 6 months weathered sample, respectively reflecting its weathering stability. It also showed some differences within other oils. Hence, this ratio can be used as a marker of the studied crude and accordingly may be applied for spilled oil source identification in such instances where the light components have already been lost due to environmental influences.     

Size characterization of the associations between carbon nanotubes and humic acids in aqueous media by asymmetrical flow field-flow fractionation combined with multi-angle light scattering

This work focuses on the influence of humic acids (HAs) on the fate of carbon nanotubes (CNTs) in aqueous media. This influence was demonstrated by mixing CNT powder with HAs in aqueous solution in varying concentrations. The aqueous media containing HAs and CNTs were size-characterized by asymmetrical flow field-flow fractionation (AsFlFFF) coupled with multi-angle light scattering (MALS). This coupling yielded information concerning the size distribution of single- and multi-walled CNTs (SWCNTs and MWCNTs) and HAs under different physico-chemical conditions that can occur in environmental water. HAs can disperse individual CNTs in aqueous media. However, the difference in the physical structure between SWCNTs and MWCNTs leads to significant differences in the quantity of HA that can adsorb onto the nanotube surface and in the stability of the CNT/HA complex. Compared with MWCNTs, SWCNTs suspended in HAs are less affected by changing ionic strength with respect to stability and the amount suspended.