Removal of carotene-like colored compounds by liquid-liquid extraction during polycyclic aromatic hydrocarbons analysis of plant tissue

Plants contain a wide variety of chemicals, some of which may have similar chromatographic behavior to polycyclic aromatic hydrocarbons (PAHs). During solid phase extraction (SPE) with Si-gel for instance, the co-elution of carotene-like colored compounds with PAHs has been observed. In this paper, liquid–liquid extraction was applied for the separation and subsequent analysis of PAHs from plant extracts. PAHs containing 2–6 rings, which include naphthalene, phenanthrene, pyrene, benzo[a]pyrene and benzo[ghi]perylene, were used as representative target chemicals. Carotene-like compounds extracted from Komatsuna (Brassica campestris) shoot by acetone followed by Si-gel treatment were incorporated as undesired components in the model matrix. Results showed the feasibility of employing either acetonitrile or 2% (w/v) KOH–methanol as solvents for high PAHs recovery and low extraction of colored fraction. For acetonitrile, 86.9–93.5% of each PAH could be recovered after three extraction cycles (relative standard deviation, RSD < 1.6%) with only about 10% co-extraction of colored fraction. For 2% KOH–methanol, PAHs recoveries ranging from 79.3% to 83.1% after five cycles (RSD < 1.5%) were achieved while the percent extraction of colored fraction was also low at 10%. The relatively higher selectivity of the solvents for PAHs over the colored fraction as well as the solubility of the matrix solution in the solvent may have contributed to these results. On this basis, liquid–liquid extraction is very useful for the pre-treatment of plant extracts for PAHs analysis.     

气相色谱法测定工作场所空气中的二甲基甲酰胺

针对毛细管柱恒温分析时色谱峰裂分和定量重复性差的问题,对色谱分析条件进行了改进,建立了不分流进样程序升温的二甲基甲酰胺气相色谱测定方法提高了柱效和样品分析的准确度,降低了检出限(检出限为0.3μg/mL)。     

不同区域城市排水系统中H2S的溢出规律

通过对广州、兰州和昆明等城市排水系统中H2S的溢出浓度、管网参数与水质指标等进行实地监测,考察不同区域城市排水系统中H2S溢出规律.结果表明,不同城市排水系统中H2S的溢出浓度与当地居民生活习惯相关,并具有明显的时段特征;在相同监测时段内,不同区域H2S溢出浓度与溶解氧浓度(DO)、有机物浓度、硫化物浓度、硫酸盐浓度以及污水流量有关.单样本K-S检验结果表明,不同区域城市排水系统H2S的溢出浓度具有相同分布规律,均近似服从正态分布.独立样本t检验结果表明,广州与兰州H2S的溢出浓度没有显著差异,但与昆明的H2S溢出浓度则具有显著差异.     

固体进样-电热蒸发-原子吸收法测定土壤中的镉

采用固体进样原子吸收法直接测定土壤中的镉,可以避免传统酸消解预处理过程耗时长、试剂消耗大、操作步骤繁琐等缺点,提升镉的检测效率。通过优化测镉仪的仪器参数,确定了固体进样-电热蒸发-原子吸收法的优化仪器条件。采用优化条件测定了不同浓度的土壤样品,研究了该方法的检出限、正确度、精密度。研究结果表明:镉质量范围为0~200 ng时与峰面积的线性相关系数优于0.999 5,空气流下优化的灰化温度和热解温度均为800 ℃,优化的热解气体氢气流量为300 mL/min,当样品进样量为0.1 g时,检出限为0.009 mg/kg,7次连续测定相对标准偏差为1.4%~5.0%,加标回收率为96.2%~102.1%,分析时间小于4 min。该方法操作简便,用时短,无需高压气源,可以用于土壤中镉的高效检测。     

一种基于小样本数据信息扩散的重大火灾频度估算方法

重大火灾的发生是小概率事件,其历史数据属于小样本统计数据。在应用频率直方图法对小样本数据进行处理时,分析结果对直方图的起点、区间步长以及样本中的奇异数据十分敏感。采用信息扩散方法,对日本1995-2008年各年重大火灾次数统计样本进行分析,对比了不同扩散条件下的扩散结果,结果表明信息扩散方法具有很好的稳定性和一致性。基于信息扩散的结果,计算了以年为周期的重大火灾发生次数的超越概率分布,建立了一种重大火灾频度估算方法。     

石蒜属植物的引种选育及快繁研究进展

石蒜属植物具有观赏、药用等利用价值。我国是石蒜属植物的主要分布区域,概述了近年来石蒜属植物在引种选育、开发利用及快速繁殖等方面的研究进展,对石蒜属未来的研究方向进行了展望,并对进一步开发利用该属植物资源提出建议。     

固相萃取-高效液相色谱法测定水中微囊藻毒素质量控制指标研究

采用固相萃取－液相色谱法,通过统计全国多家实验室的测定数据,对水中微囊藻毒素测试的平行样测定相对偏差、空白加标回收率、实际样品加标回收率、空白加标回收率平行样相对偏差以及样品加标回收率平行样相对偏差5个质控指标进行了研究,并给出了质控指标评价标准,提出在概率P和γ均为0.90时,其平行样测定允许最大相对偏差应控制在7.3%;空白加标质量浓度为0.005~20 μg/L时,回收率的控制范围为61%~125%;样品测定浓度为未检出、加标质量浓度在0.2~3.6 μg/L时,实际样品加标回收率控制范围为66%~108%;空白加标、样品加标回收率平行样最大相对偏差应分别控制在3.9%和8.9%。在概率P和γ均为0.95时,其平行样测定允许最大相对偏差应控制在8.3%;空白加标质量浓度为0.005~20 μg/L时,回收率的控制范围为49%~137%;样品测定浓度为未检出、加标质量浓度在0.2~3.6 μg/L时,实际样品加标回收率控制范围为60%~114%;空白加标、样品加标回收率平行样最大相对偏差应分别控制在5.2% 和14.8%。     

Determination of Water-soluble Atmospheric Aerosols Using Ion Chromatography

A field study was established to investigate the chemical composition of atmospheric aerosols in Chicago, IL. One goal of this study was to determine the influence of precursor trace gases and local meteorology on concentrations of secondary aerosol ionic species. This paper describes the method details, shows the method is analytically valid, and reports overall as well as some specific results found during the field study. Two particulate air samples were collected per day onto quartz fiber filters at the Loyola University Chicago Air Station during the summer months in 2002–2004. In parallel, mixing ratios of ozone and nitrogen oxides were monitored and weather parameters were recorded. Particulates were extracted from the filter substrates and the subsequent solutions were analyzed by ion chromatography for anions, including low molecular weight organic acids, and cations. A washing procedure was implemented to reduce the high background values of the quartz fiber filters. Method validation showed that the collection method was efficient for all ions with exception of nitrate, whose efficiency of 70% indicated losses caused by volatilization. The extraction method also proved efficient for both field and laboratory samples, and the repeatability of the method was high with relative standard deviations less than 10% for all ions. Reproducibility of the results was determined by comparison of sulfate to sulfur analyzed by total reflection X-ray fluorescence spectrometry and proved to be high as well. Concentrations differed significantly between the three summer studies due to varying levels of precursor species as a consequence of distinct temperatures and wind direction profiles.     

Volatile organic chloramines formation during ClO2 treatment

Volatile organic chloramines are reported as the disinfection byproducts during chlorination or chloramination.However,ClO_2,as an important alternative disinfectant for chlorine,was not considered to produce halogenated amines.In the present work,volatile organic chloramines including(CH_3)_2 NCl and CH_3 NCl_2 were found to be generated during the reaction of ClO_2 and the dye pollutants.(CH_3)_2 NCl was the dominant volatile DBP to result from ClO_2 treated all four dye pollutants including Methyl Orange,Methyl Red,Methylene Blue and Malachite Green,with molar yields ranging from 2.6% to 38.5% at a ClO_2 to precursor(ClO_2/P) molar ratio of 10.HOCl was identified and proved to be the reactive species for the formation of (CH_3)_2 NCl,which implied(CH_3)_2 NCl was transformed by a combined oxidation of ClO_2 and hypochlorous acid.(CH_3)_2 NCl concentrations in the ppb range were observed when real water samples were treated by ClO_2 in the presence of the dye pollutants.The results suggest that these azo dyes are one of the significant precursors for the formation of HOCl during ClO_2 treatment and that organic chloramines should be considered in ClO_2 disinfection chemistry and water treatment.     

浅议现代垃圾填埋场的大气污染及监测分析方法

造成垃圾填埋场大气污染的两大类污染物,其对环境、人体、动植物、器物和材料都有一定的危害,文章针对现代垃圾填埋场的大气环境污染,以硫化氢、氨、甲硫醇等重点大气污染因子为监测对象,结合实践总结了一部分垃圾填埋场的大气污染监测方案,包括布点原则、采样频率和时间、采样方法和分析技术,该监测方案可为现代垃圾填埋场的大气污染监测提供参考.