Improvement of an efficient separation method for chemicals in diesel exhaust particles: analysis for nitrophenols

GOAL, SCOPE, AND BACKGROUND: Diesel exhaust is believed to consist of thousands of organic constituents and is a major cause of urban pollution. We recently reported that a systematic separation procedure involving successive solvent extractions, followed by repeated column chromatography, resulted in the isolation of vasodilatory active nitrophenols. These findings indicated that the estimation of the amount of nitrophenols in the environment is important to evaluate their effect on human health. The isolation procedure, however, involved successive solvent extractions followed by tedious, repeated chromatography, resulting in poor fractionation and in a significant loss of accuracy and reliability. Therefore, it was crucial to develop an alternative, efficient, and reliable analytical method. Here, we describe a facile and efficient acid-base extraction procedure for the analysis of nitrophenols. MATERIALS AND METHODS: Diesel exhaust particles (DEP) were collected from the exhaust of a 4JB1-type engine (ISUZU Automobile Co., Tokyo, Japan). Gas chromatography-mass spectrometry (GC-MS) analysis was performed with a GCMS-QP2010 instrument (Shimadzu, Kyoto, Japan). RESULTS: A solution of DEP in 1-butanol was extracted with aqueous NaOH to afford a nitrophenol-rich oily extract. The resulting oil was methylated with trimethylsilyldiazomethane and subsequently subjected to GC-MS analysis, revealing that 4-nitrophenol, 3-methyl-4-nitrophenol, 2-methyl-4-nitrophenol, and 4-nitro-3-phenylphenol were present in significantly higher concentrations than those reported previously. DISCUSSION: Simple acid-base extraction followed by the direct analysis of the resulting extract by GC-MS gave only broad peaks of nitrophenols with a poor detection limit, while the GC-MS analysis of the sample pretreated with (trimethylsilyl)diazomethane gave satisfactorily clear chromatograms with sharp peaks and with a significantly lowered detection limit (0.5 ng/ml, approximately 100 times). CONCLUSION: The present method involving an acid-base extraction, in situ derivatization, and GC-MS analysis has shown to be a simple, efficient, and reliable method for the isolation and identification of the chemical substances in DEP.     

Pb/Zn冶炼废渣中重金属的生物浸出-盐浸处理

利用中温嗜热菌对某铅锌冶炼废渣进行生物浸出盐浸处理研究,并根据国家固体废物浸出毒性方法(HJ/T299-2007)对盐浸后余渣进行毒性分析。研究结果表明,在pH 1.5、温度65℃、矿浆浓度5%的优化条件下生物浸出3 d后,废渣中Cu、In、Ga和Zn的浸出率分别达到了91.5%、91.8%、84.9%和93.4%;盐浸生物浸出渣,其浸出液中Ag、Pb浓度分别为7.6和247.5 mg/L,可从废渣中有效回收Cu、In、Ga、Zn、Ag和Pb。生物浸出盐浸处理后余渣约为原渣量的70%;毒性分析浸出液中重金属元素Ag、As、Cd、Cu、Pb和Zn浓度分别为2～3.5、2～3、0.3～0.5、30～50、2～4、20～60 mg/L,低于国家危险废物鉴别标准(GB5085.3-2007)。根据试验结果,提出了针对冶炼废渣资源化、减量化、无害化的生物浸出盐浸联用工艺。     

GC/MS法测定黄浦江水中挥发性有机化合物

采用吹扫捕集装置与GC／MS联用仪的全自动恒流控制,对黄浦江7个断面水样中47种挥发性有机化合物进行了分析。结果表明,被查的47种挥发性有机化合物基本都有检出,其中甲苯、异丙苯的绝对检出量最高。四氯化碳的检出值也较高,吴淞口四氯化碳的平均浓度已经远远超过GB3838—2002《地表水环境质量标准》,并且四氯化碳浓度在黄浦江流域各个断面的分布具有一定规律性。     

便携式GC-MS法快速测定固定污染源废气中的VOCs

采用便携式GC-MS法快速测定固定污染源废气中VOCs,32种VOCs在2×10~(-7)~1×10~(-6)范围内线性良好,方法检出限为2×10~(-9)~1×10~(-8),标准气体样品6次测定结果的RSD为1.9%~19.1%,环境空气样品的加标回收率为66.2%~116%。在实际现场监测固定污染源中VOCs时,使用速查(Survey)功能可初步判断样品浓度,确定稀释倍数。比对试验结果表明,气袋和玻璃注射器采样法对VOCs测定结果无显著性差异。     

二氧化铅电极的制备、表征及其电催化性能研究

以电沉积法制备了Ti/PbO2和Ti/MnO2/PbO22种电极.采用SEM、XRD和XPS等分析方法表征了电极的形貌、元素组成及元素化学态,并以罗丹明B为目标有机物,考察了所制备电极的析氧极化曲线和电催化活性以及Ti/MnO2/PbO2电极的循环伏安曲线.研究结果表明,Ti/MnO2/PbO2电极的稳定性、使用寿命、析氧电位和电催化活性较Ti/PbO2电极都有所提高,并且罗丹明B在Ti/MnO2/PbO2电极上的反应主要发生在析氧反应区,且反应不可逆.     

纯种氨氧化菌短程反硝化特性

以Comamonas aquatica LNL3为研究对象,根据其既能短程硝化又能短程反硝化的特性,采用好氧方式富集和固定化菌种,再以厌氧方式驯化,得到具有高效短程反硝化特性的纯种氨氧化菌。采用扫描电镜对固定化前后的载体进行表征,且用正交试验考察了不同环境因子(温度、pH、碳氮比、溶解氧)对Comamonas aquatica LNL3短程反硝化的影响。结果表明,所用载体与Comamonas aquatica LNL3有良好的亲和性,适于微生物的固定化;环境因子对Comamonas aquatica LNL3短程反硝化影响大小顺序为:温度>pH>DO>C/N;在环境条件改变过程中当温度为35℃,pH=8,C/N=3,DO=2.5 mg/L时,Comamonas aquatica LNL3短程反硝化速率达到最大,为32.63 mg/(L.h);研究结果还表明,Comamonas aquatica LNL3具有好氧反硝化特性,适宜处理低碳氮比废水。     

吹扫捕集与气相色谱-质谱联用测定饮用水和地表水中挥发性有机污染物

报道了Trap I(VOCARB 4000)柱捕集水中挥发性有机污染物的性能和条件,建立了吹扫捕集和气相色谱-质谱联用测定饮用水和地表水样中25种挥发性有机污染物的分析方法.水样的加标回收率在90%～110%之间,最低检测限在0.04～0.85μg/L之间,20μg/L的挥发性有机物标准溶液经重复6次测定,其相对标准偏差基本小于5.0%.该方法已成功地运用于饮用水和地表水中挥发性有机污染物的测定,结果令人满意.     

纳米ZnO/PS薄膜的制备及光降解性能

利用纳米ZnO与聚苯乙烯(PS)高速共混法制备了一种在紫外光下具有自降解性能的复合薄膜.分析表明,经过KH570处理的纳米ZnO与PS通过化学键的方式桥联在一起.TG分析表明,复合薄膜的耐热性较PS有所提高;SEM图像显示0.5 wt％ ZnO在PS薄膜表面分布均匀,经过UV照射后薄膜表面出现光腐蚀现象.复合薄膜紫外光自降解实验表明:0.5 wt％ ZnO/PS薄膜在15W的紫外灯照射下,15d的自降解率为3.715％.     

Ti/BDD/PbO_2复合电极在化学需氧量测定中的应用

以钛基掺硼金刚石为基体,采用电沉积的方法制备了Ti/BDD/PbO2复合电极,并将其用于化学需氧量（COD）的测定。采用扫描电子显微镜（SEM）和X射线衍射谱图（XRD）表征了电极的微观形貌及结构,采用电化学工作站考察了电极对有机物响应特性。实验结果表明,在1.45 V的低电位条件下,线性范围为0.5～175 mg/L,检测限为0.3 mg/L（S/N=3）。采用Ti/BDD/PbO2复合电极测定法和重铬酸钾标准方法对市政污水、食品废水及印染废水的对比结果表明,2种方法的相对误差小于10%,具有良好的一致性。     

基于O/E模型的浅水湖泊生态系统健康评价

以长江中下游阻隔型浅水湖泊为研究对象,分析了1998—2018年116湖次底栖动物野外调查数据,构建了基于预测模型的观测物种组成/期望物种组成(O/E)指数健康评价指标体系,评价了长江中下游浅水湖泊的底栖动物物种组成完整性.O/E指数模型评价结果显示,在物种采集概率(Pc)>0阈值条件下的O/E0模型预测得到的监测湖泊...