北京地区大气颗粒物中有机物的分析

报告了一年四个季节组合样品中的有机成分分析结果。GC/MS定性分析表明,颗粒物有机物可抽提部分中,可分析识别的主要种类有正构烷烃、脂肪酸、多环芳烃等。其中正构烷烃有明显的奇数碳优先,而脂肪酸有明显的偶数碳优先。GC定量分析正构烷烃的结果和HPLC定量分析多环芳烃的结果均显示,天坛站点的有机物污染浓度大于十三陵站点。污染水平秋冬季高,春夏季低,这种季节变化趋势与有机碳总量相同。      

Biodegradation of triazine herbicide metribuzin by the strain Bacillus sp. N1

By enrichment culturing of soil contaminated with metribuzin, a highly efficient metribuzin degrading bacterium, Bacillus sp. N1, was isolated. This strain grows using metribuzin at 5.0% (v/v) as the sole nitrogen source in a liquid medium. Optimal metribuzin degradation occurred at a temperature of 30ºC and at pH 7.0. With an initial concentration of 20 mg L^?1, the degradation rate was 73.5% in 120 h. If the initial concentrations were higher than 50 mg L^?1, the biodegradation rates decreased as the metribuzin concentrations increased. When the concentration was 100 mg L^?1, the degradation rate was only 45%. Degradation followed the pesticide degradation kinetic equation at initial concentrations between 5 mg L^?1 and 50 mg L^?1. When the metribuzin contaminated soil was mixed with strain N1 (with the concentration of metribuzin being 20 mg L^?1 and the inoculation rate of 10¹¹ g^?1 dry soil), the degradation rate of the metribuzin was 66.4% in 30 days, while the degradation rate of metribuzin was only 19.4% in the control soil without the strain N1. These results indicate that the strain N1 can significantly increase the degradation rate of metribuzin in contaminated soil.     

碱性微波提取-ICP/MS法测定土壤中六价铬

采用碱性微波提取法处理土壤样品,用电感耦合等离子体质谱（ICP/MS）法测定试样中的六价铬,以标准物质测定相对误差的绝对值作为试验指标建立正交模型,确定碱性微波消解的提取温度95 ℃、提取时间30 min、氯化镁用量005 g、提取液体积6 mL为最佳试验条件,采用He碰撞池技术和在线内标分别消除基体带来的质谱和非质谱干扰。条件优化后,方法检出限为0.10 mg/kg,实际样品6次测定结果的RSD分别为13.0%和5.7%,加标回收率为120%和106%。将该方法用于有证标准土壤样品的测定,测定结果均在标准值范围内。     

Simultaneous determination of gaseous and particulate chlorinated polycyclic aromatic hydrocarbons in emissions from the scorching of polyvinylidene chloride film

An analytical method for the determination of gaseous and particulate chlorinated polycyclic aromatic hydrocarbons (ClPAHs) was investigated. By means of this method, concentrations and isomer profiles of the 27 target ClPAHs could be analyzed. To evaluate the usefulness of the method for analyzing ClPAH emissions, laboratory-scale scorching tests were performed on polyvinylidene chloride (PVDC) plastic wrap over a flame of the gas burner. Only seven of the target ClPAHs were detected, and all compounds detected had 2, 3, or 4 rings. The detected ClPAHs were present in both the particulate phase and the gaseous phase, but they were present at higher concentrations in the gaseous phase than in the particulate phase. Relationships between the number of chlorine substituents on the naphthalene/phenanthrene rings and the overall concentration and the percentage in the particulate phase were also investigated.     

Rapid detection of multiple class pharmaceuticals in both municipal wastewater and sludge with ultra high performance liquid chromatography tandem mass spectrometry

This work described the development, optimization and validation of an analytical method for rapid detection of multiple-class pharmaceuticals in both municipal wastewater and sludge samples based on ultrasonic solvent extraction, solid-phase extraction, and ultra high performance liquid chromatography-tandem mass spectrometry quantification. The results indicated that the developed method could effectively extract all the target pharmaceuticals （25） in a single process and analyze them within 24 min. The recoveries of the target pharmaceuticals were in the range of 69%-131% for wastewater and 54%-130% for sludge at different spiked concentration levels. The method quantification limits in wastewater and sludge ranged from 0.02 to 0.73 ng/L and from 0.02 to 1.00μg/kg, respectively. Subsequently, this method was validated and applied for residual pharma- ceutical analysis in a wastewater treatment plant located in Beijing, China. All the target pharmaceuticals were detected in the influent samples with concentrations varying from 0.09 ng/L （tiamulin） to 15.24 μg/L （caffeine）; meanwhile, up to 23 pharmaceuticals were detected in sludge samples with concentrations varying from 60 ng/kg （sulfamethizole） to 8.55 mg/kg （ofloxacin）. The developed method demonstrated its selectivity, sensitivity, and reliability for detecting multiple-class pharmaceuticals in complex matrices such as municipal wastewater and sludge.     

钱塘江(杭州段)表层水中全氟化合物的残留水平及分布特征

为探究钱塘江(杭州段)表层水中全氟化合物(PFCs)的污染特征,应用固相萃取净化、富集与超高效液相色谱-串联质谱联用相结合的方法,对14个监测断面采集于2014年7月和2015年1月的表层水样品中16种PFCs进行了分析,研究其残留水平和分布规律.监测结果显示钱塘江(杭州段)表层水有8种PFCs不同程度的检出,包括C4和C8全氟烷基磺酸以及C4~C9全氟烷基羧酸,均为中短链PFCs.ΣPFCs质量浓度范围为0.98~609 ng·L~(-1),其中全氟辛酸(PFOA)质量浓度范围0.59~538 ng·L~(-1),为主要污染因子,全氟辛烷磺酸(PFOS)检出浓度较低,为0~2.48 ng·L~(~(-1)).污染物空间分布略有差异,位于上游兰江的兰江口和将军岩断面检出浓度较高,总体上呈现上游高于下游的趋势.特征组分含量比率显示流域内工业污废水排放是水体中PFCs残留的主要来源.钱塘江(杭州段)水体中PFCs污染与钱塘江流域上游产业布局密切相关,主要污染输入来自上游兰江,沿途吸纳的含PFCs的污废水对水体污染有一定影响.研究结果表明钱塘江水体中存在着广泛的PFCs特别是PFOA污染,需要有关部门引起足够的重视.     

吹扫捕集-GC／MS联用定性分析城镇污水处理厂难降解污染物研究

采用吹扫捕集-GC／MS法对浙江省某工业园区污水处理厂中残留的难降解物质进行了定性和半定量分析,分析结果有9个响应值较高的峰,通过NIST库检索,得到这9个物质在水中残留的浓度高低依次是二氯甲烷最高,其次是四氢呋喃、三氯甲烷、1,4-二氯苯、1,2-二氯乙烷、二甲氧基甲烷、五氯环丙烷、1,4-二氯-2-氟苯、N,N-二甲基苯胺。并从这几种物质的性质、用途和这个工业园区生产企业生产的产品,分析了这几种物质在这个工业园区污水中残留的原因及危害,同时提出去除这些残留物质的方法。     

气相色谱氮磷检测器法测定饮用水中19种苯胺类化合物

建立了气相色谱氮磷检测器法(GC-NPD)测定饮用水中19种苯胺类化合物。结果表明,19种苯胺类化合物的方法检出限在0.06⁰.45μg/L之间,其线性定量范围均为0.050.45μg/L之间,其线性定量范围均为0.05¹0.0 mg/L,相关系数(R)在0.995 110.0 mg/L,相关系数(R)在0.995 1⁰.999 8之间;方法平均加标回收率在70.7%0.999 8之间;方法平均加标回收率在70.7%¹08.2%之间,RSD(n=6)为2.9%108.2%之间,RSD(n=6)为2.9%¹8.5%。该法灵敏度高,快速准确,用于实际水样测定的结果令人满意。     

电感耦合等离子法测定环境积尘中铅的研究

用细毛刷清扫收集普通居民房顶积尘,参照土壤样品预处理方法-普通酸分解法处理样品,以国标样品、不确定度实验、加标回收实验为质控手段,探索采用电感耦合等离子法测定环境积尘中铅的含量。实验结果表明,该法能将积尘样品完全消解,且电感耦合等离子法测试方法性能稳定、快速、准确,优于其他方法。     

气相色谱法、气质联用法测定土壤中多氯联苯

采用快速溶剂萃取法提取土壤中的7组多氯联苯Aroclors系列,经弗罗里硅土柱净化,用气相色谱／电子捕获检测器法（GC／ECD）和气质联用法（GC／MS）进行测定。当取样量为20g时。GC／ECD法和GC／MS法的检出限分别为0．28～0．87μg／kg和0．62～1．35μg／kg。两种方法的基体加标回收率在79．6％--103．6％,相对标准偏差〈9．0％。利用该方法分析Aroclor有证土壤标样,结果满意。GC／ECD法的准确度和精密度略优于GC／MS法,因此实际土壤样品Aroclors分析中,建议以GC／ECD的定量结果为准。