A gas chromatography/mass spectrometry method for the simultaneous analysis of 50 phenols in wastewater using deconvolution technology

Phenolic compounds exist widely in the influents and effluents of sewage treatment plants (STPs) and most are un-regulated. In this study, a gas chromatography-mass spectrometry (GC-MS) method for the simultaneous analysis of 50 phenolic compounds in wastewater was developed. Deconvolution technology was used to identify contaminants that are covered by co-extracted materials. A mass spectral library containing all 50 silylated phenolic compounds was first established and used for deconvolution. Twelve typical phenolic compounds were selected to optimize the sample preparation procedures. Solid-phase extraction using a C18 cartridge coupled with an HLB cartridge was used for pre-concentration and dichloromethane was used for elution. The solutes were derivatized and analyzed by GC-MS. The blank and matrix spike recoveries ranged from 57.46% to 136.4% and 47.87% to 114.8%, respectively. Method detection limits ranged from 3.64 to 97.64 ng L⁻¹. The relative standard deviations of all the recovery experiments were lower than 13.6%. The instrument limits of quantification ranged from 0.7 to 87.7 pg. The method has been applied to analyze the influents and effluents of 5 Chinese STPs. Except for regulated phenolic compounds (phenol and 2,4,6-trichlorophenol), three un-regulated phenolic compounds, including 2-chlorophenol, 2,5-dichlorophenol and 2,4-dichloro-3-ethyl-6-nitrophenol were identified in the effluent wastewater. The detected concentrations of un-regulated phenolic compounds could possibly cause environmental effects, indicating that immediate attention is required to prevent complications.     

超声辅助萃取-高效液相色谱法测定牛奶中9种β-内酰胺抗生素残留

 建立了一种采用超声辅助萃取-高效液相色谱法检测牛奶中9种β-内酰胺抗生素残留的方法.牛奶样品经过乙腈沉淀蛋白,磷酸盐缓冲溶液为提取液,20kHz超声处理5min,离心处理,固相萃取小柱净化,采用Agilent TC C18 (150mm×4.6mm,5μm)色谱柱,选用磷酸盐-甲醇作流动相进行梯度洗脱,流速1.0mL/min,220nm检测,在22min内分离检测.方法可用于牛奶中上述抗生素残留的同时检测.     

炼油厂废水库底泥中半挥发性有机污染物监测与评价

采用超声提取结合GC/MS测定了克拉玛依炼油厂污水库底质中的半挥发性有机物。选择16个多环芳烃作为加标物,测定超声提取法的回收率在65%94%。从底泥中检出62个色谱峰,能准确定性20个组分,主要包括9个多环芳烃、5个正构烷烃和3个酚类化合物。对缺少标准物的组分采用结构相似物进行定量,浓度范围在0.1259 ng/g。...     

和田茴香籽中黄酮类化合物提取工艺研究

采用正交设计法对新疆和田茴香籽中的黄酮类化合物提取工艺参数进行优化.结果表明:最佳提取工艺为70 ml 60％乙醇在70℃下提取2.5h.本实验采用分光光度法,以芦丁标准品测定新疆和田茴香籽提取物中总黄酮的含量,总黄酮含量为1.58％.该工艺稳定、简便、快速,可作为检测茴香籽提取物中黄酮含量的一种手段.     

物理气相传输(PVT)法生长碳化硅的晶体形态热应力分析

利用有限元方法对物理气相传输(PVT)法生长碳化硅晶体过程中出现的3种典型生长形态进行了热应力分析.结果表明:在3种晶体生长形态中,热应力最大值都出现在晶体与石墨坩埚盖接触区域;平面型生长形态中温度场及相应的热应变场和等效应力场分布均比较均匀;凸面型和凹面型生长形态的温度场及相应的热应变场和等效应力场分布均变化较大,而且在凸面型的中间区域和凹面型的边缘区域也存在较大的应力值.因此,为提高晶体质量,提出在石墨坩埚盖上沉积或反应生成碳化硅过渡层来减小热应力的改良方法,同时调整碳化硅晶体生长系统,尽量保证碳化硅晶体的平面型生长形态.     

基于曲波变换和Susan种子点生长的边缘检测算法

针对现存的基于空间域的图像边缘检测算法只能有效检测出图像有限方向边缘以及对于纹理复杂的图像边缘定位困难等问题,提出了一种基于曲波变换和Susan种子点生长的边缘检测算法,该算法首先对源图像进行曲波变换,然后对高频子图像运用Susan种子点生长算法进行边缘提取;对低频子图像采用极大值方法将轮廓检测出来,最后通过一定的融合...     

GIS环境下基于GDEM的丹江口库区流域自动提取方法的研究

小流域是一个相对完整的生态过程单元,以小流域为研究单元,可以从中观尺度认识库区的地理规律,从而推动库区的生态环境治理和生态环境建设.研究区域选择丹江口库区,以30 m分辨率的DEM为数据源,采用ESRI公司开发的ArcGIS软件,研究流域的自动提取的方法.先对DEM数据进行填洼和削峰的预处理;再经过水流方向的确定,汇流...     

关联维数的超声波电机故障诊断

利用关联维数分析方法对超声波电机进行故障诊断,并针对故障诊断的实际情况,建构特殊实验平台采集故障振动信号.通过互信息法及Cao方法来确定相空间重构的2个重要参数,然后计算超声波电机在不同故障状态下的关联维数.结果表明,不同故障状态产生机制不同,其关联维数也不同,关联维数可用于故障的特征提取.通过分析不同状态下超声波电机...     

用改进的酚-氯仿法提取榕小蜂基因组DNA及SRAP分析

以传粉榕小蜂为材料,用改进的酚-氯仿法对不同保存条件下的样品提取基因组DNA,并进行分光光度、琼脂糖凝胶电泳、SRAP扩增等方法的鉴定.结果表明:改进的酚-氯仿法均可从4种保存条件下的样品中提取出DNA,新鲜样品和体积分数95％乙醇固定样品提取效果比其他2组提取效果好.选择体积分数95％乙醇固定所提取的DNA为模板进行...