液膜法提取水溶液中的苯胺

本文研究了用煤油－磷酸三丁酯－Ｓｐａｎ８０－脂肪酸酯－ＨＣｌ溶液制成的液膜体系从水中溶液中提取苯胺的过程。并对溶剂和表面活性剂的选择及用量,搅拌速度,Ｒｉｅ,Ｒｅｗ,外相ｐＨ的选择进行了和系列的研究。结果表明,该法既适用于高浓度又适于低浓度的苯胺水溶液的处理。     

Determination of phenolic and steroid endocrine disrupting compounds in environmental matrices

BACKGROUND, AIM AND SCOPE: Many pollutants have received significant attention due to their potential estrogenic effect and are classified as endocrine disrupting compounds (EDCs). EDCs comprise many classes of organic compounds. The development or optimization of analytical protocols for the simultaneous determination of EDCs in environmental samples is an analytical challenge because these compounds exhibit different physicochemical characteristics, they occur in the aquatic environment in relatively low concentrations and, furthermore, environmental samples are considered as complex matrices. The aim of this study is the development of analytical methods for the simultaneous determination of phenolic and steroid EDCs in aqueous and solid samples. The target compounds are 4-nonylphenol, 4-octylphenol, their ethoxylate oligomers (mono- and di-ethoxylates of nonylphenol and octylphenol), bisphenol A, the estrogens (estriol, estrone, 17beta-estradiol, 17alpha-estradiol) and the synthetic steroids (mestranol and 17alpha-ethynylestradiol). MATERIALS AND METHODS: Solid phase extraction employing Oasis HLB cartridges and different elution solvents was used for the recovery studies of the target compounds from various types of water samples (ultrapure water, artificial seawater, river water and seawater). Ultrasonic assisted extraction was applied for the recovery of the target EDCs from the solid samples. The recoveries were assessed using various solvents for the extraction and the elution of EDCs from different SPE cartridges used for clean up. Gas chromatography-mass spectrometry after derivatization with N,O-bis(trimethylsilyl)-trifluoroacetamide was employed for the determination of these compounds. RESULTS AND DISCUSSION: The recovery rates of three elution solvents (methanol, acetone and ethylacetate) for the extraction of target EDCs from artificial seawater were assessed after preconcentration on SPE cartridges. Acetone showed better recoveries and was further tested for its extraction efficiency in different water types (river water, seawater). Ultrasonic assisted extraction was used for the recovery of target EDCs from solid matrices. Acetone, methanol, mixture of acetone-methanol (1:1) and ethylacetate were used as extraction solvents. Ethylacetate and the mixture of acetone-methanol (1:1) exhibited better extraction efficiencies. An additional clean up step was necessary for sediment samples. Different SPE cartridges were employed for clean up of the extracts (Oasis HLB, C18, Florisil, silica, combination of silica and alumina). Florisil cartridges were finally used. The proposed methods were further validated on the determination of target EDCs in field collected samples (river water, seawater, wastewater, total suspended solids and sediments) from the major area of Thessaloniki, Greece. CONCLUSIONS: Efficient and accurate integrated methods for the simultaneous determination of alkylphenols (nonylphenol, octylphenol), their ethoxylate oligomers (mono- and di-ethoxylate of nonylphenol and octylphenol), bisphenol A and steroids (estriol, estrone, 17beta-estradiol, 17alpha-estradiol, mestranol and 17alpha-ethynylestradiol) in aqueous and solid samples were developed. The proposed methods were applied for the determination of the target compounds in representative environmental samples in the area of Thessaloniki, Northern Greece. RECOMMENDATIONS AND PERSPECTIVES: This study confirms the occurrence of selected EDCs in inland and marine waters in the area of Thessaloniki, Northern Greece. Since there is no previous data on the occurrence of the target EDCs in the major area, an extended survey is in progress to evaluate the occurrence and fate of these compounds.     

土壤气相抽提法去除红壤中挥发性有机污染物的影响因素研究

土壤气相抽提技术(SVE)是一种安全、经济、高效的土壤治理技术,广泛应用于不饱和土壤中挥发性有机污染物的去除.本实验以我国南方典型土壤红壤(粘性较大的土壤)为实验土样,选用最常见的挥发性有机物苯作为污染物,采用一维土柱通风模拟SVE过程,研究了通风流量、土壤含水率以及间歇操作对苯污染红壤去污过程的影响.结果表明,在各土柱垂向气相中苯浓度变化趋势一致,通风初期浓度迅速降低后进入长时间的拖尾阶段,拖尾阶段初期进行间歇操作可降低能耗达到较经济的治理效果.通风流量与土壤含水率是影响净化时间和修复效果的重要因素,两者均存在最佳值.当通风流量为600 mL/min,含水率为17.2%时本实验净化时间降低为36 h,去除率为99.9%,达到了最佳的治理效果.     

连续流动-固相微萃取方法富集水中多环芳烃的探讨

建立了连续流动-固相微萃取富集、气相色谱测定水中多环芳烃的方法,探讨了流量和溶液体积对萃取效果的影响。方法在0μg／L-40μg／L范围内线性良好,8种多环芳烃的检出限为0．05μg／L-0．5μg／L,样品测定的相对标准偏差〈7％,加标回收率为87．0％～112％。     

天冬氨酸和柠檬酸对污泥中重金属萃取的比较研究

以天冬氨酸作为萃取剂,研究了其对上海桃浦污水处理厂污泥中重金属的萃取性能,重点考察了萃取体系pH值对重金属萃取的影响,并在相同条件下与柠檬酸的萃取过程进行比较.结果表明,随着萃取体系pH值的升高,重金属的萃取率逐渐降低.在较低pH值时,天冬氨酸对污泥中Zn、Ni及Cu的最高萃取率均大于85%;在整个实验pH值范围内,天冬氨酸对Ni及Cu的萃取率分别达到50%和40%以上.与柠檬酸对污泥中上述3种重金属的萃取结果相比较,天冬氨酸对Ni、Cu的萃取能力更高,而对Zn的萃取能力在pH≥3.0时不如柠檬酸.     

聚环氧琥珀酸对污泥中铅的萃取研究

以上海市桃浦污水厂污泥为对象,研究了易生物降解的聚环氧琥珀酸(PESA)对污泥中重金属Pb的萃取作用,重点考察了萃取体系的pH值和萃取剂PESA的用量对重金属Pb萃取的影响.研究发现,PESA对污泥中的重金属Pb具有较好的萃取效果,形态分析结果表明,被PESA萃取的锌主要来自水溶态、酸溶态、可还原态和可氧化态4种形态.当萃取体系的pH=4且PESA与污泥中重金属总量的摩尔比为4∶1时,Pb的萃取效率可达73%.实验结果还表明,萃取体系的pH值和PESA用量是影响污泥中Pb萃取的重要因素.随着萃取体系pH值的降低,Pb的萃取效率总体呈现逐渐下降的趋势;随着PESA用量的增加,Pb的萃取效率逐渐提高,且对体系pH值的依赖性减小.     

混沌理论在河流溶解氧预测中的应用初探

基于混沌理论、相空间重构思想和嵌入理论分析涟水流域溶解氧的时间序列，计算吸引子维数和最大的Lyapunov指数，研究河流水质系统的复杂性特征。结果表明，河流溶解氧时间序列具有混沌特性，其外在表现为貌似随机的无规则特点；但系统本身内在的、固有的规律(表现在最大的Lyapunov指数)，表明短期预测河流水质变化是可行的，并应用混沌相空间模线性回归模型进行了预测，其预测结果对涟水流域的水质管理和控制具有一定的参考价值。     

三相流化床中混合载体的协同作用

在侧边沉降的三相气提升流化床反应器中使用粗粒焦炭和细粒石英砂混合构成载体来处理废水具有良好的协同作用。处理焦化废水的实验表明,与单一载体相比,混合载体不易流失;ＣＯＤ容积负荷高达１１ｋｇ／（ｄ·ｍ３）;对酚氰等有害物质的耐冲击能力好;高负荷运行时酚和氰的出水浓度仅为单一载体的１／５－１／３;使用混合型载体还有利于挂膜和降低曝气能耗。     

污泥胞外聚合物的提取方法及其对污泥脱水性能的影响

采用7种不同方法提取污泥胞外聚合物(EPS),并研究污泥不同层EPS剥离前后对污泥脱水性能的影响.结果表明,甲醛+NaOH和2%EDTA提取法对污泥中紧密结合的胞外聚合物(tightly bound extracellular polymeric substances,TB-EPS)提取效率最高,总固体(SS)中的EPS提取量分别为128.9 mg.g-1和42.38 mg.g-1,但提取后细胞破裂严重,不能代表污泥EPS的真实含量,不宜采用.加热法较为温和,提取效率较高,总SS中EPS产量为21.97 mg.g-1.污泥剥离黏液层(Slime层)、松散结合的胞外聚合物(loosely bound extracellular polymeric substances,LB-EPS)和TB-EPS层后污泥的脱水性能大幅度改善,其中Slime层EPS含量越高污泥的脱水性能越差,当污泥EPS大量地释放到溶液中即Slime层时污泥的CST值大幅度升高,污泥的脱水性能变差.石湖墟和昂船舟污泥初始的毛细吸水时间(CST)为132.9 s和229.9 s,当剥离Slime层时这2种污泥的CST值分别为80.8 s和79.4 s,脱水性能得到明显改善.     

固相微萃取-液相色谱法测定水中二苯并噻吩

分别采用高效液相色谱与固相微萃取-高效液相色谱法建立了水中微量二苯并噻吩的分析方法,结果表明固相微萃取对二苯并噻吩具有非常明显的富集作用。实验得到固相微萃取技术最佳检测条件为:吸附时间20min,解析时间3min,色谱流动相甲醇/水=90/10,方法的变异系数为2.85%,加标回收率102.4%,检测限0.03μg/mL。