同步衍生超声乳化微萃取气相色谱法测定环境水样中的苯胺类化合物

本研究建立了一种针对环境水样中苯胺类化合物检测的新方法——同步衍生超声乳化微萃取气相色谱法(SDUSAEME-GC-FID).通过氯甲酸丁酯(作为衍生剂/萃取相)的用量、超声时间、样品溶液p H值、离子强度和离心条件等因素对衍生/萃取效果影响的实验研究,确定了最优条件的关键性控制参数.结果表明,在选定条件下分析测定环境水样中5种苯胺类化合物,在6~60 000μg·L-1浓度范围内线性良好,相关系数R2为0.999 7~0.999 9,检测限LOD(3倍信噪比)为1.1~4.1μg·L-1,相对标准偏差RSD(n=6)为2.4%~5.7%,富集系数EF为317~846,测定7种实际环境水样的相对回收率RR为86.8%~105.5%.本方法具有操作简便、灵敏度高、经济环保的特点,可以作为检测环境水样中苯胺类化合物的一种首选方法.     

TEA滤膜挂片测定NO2用于山东省城市空气监测优化布点的研究

采用TEA滤膜挂片测定空气中NO2相对浓度的无动力采样方法，实验结果表明：TEA挂片可以反映环境空气中NO2的浓度水平，精密度较好，无需仪器、设备投入，应用于山东省15城市环境空气监测优化布点的网格实测，效果理想。     

温度对现场荧光法测定水体中叶绿素a的影响

基于高温条件下叶绿素a易降解的性质,分别以纯品叶绿素a和活体藻为实验对象探讨了温度对荧光法测定叶绿素a的影响程度及影响机理。结果显示,温度升高会提高叶绿素a的降解率,在一定温度范围内叶绿素a的相对荧光强度与温度呈良好的负线性相关;首次计算导出了叶绿素a、斜生栅藻、蛋白核小球藻及铜绿微囊藻的温度系数分别为0.30%、1.09%、1.17%及1.14%;此外,验证了在现场测定中当环境温度为15~35℃时温度对水体叶绿素现场检测仪的影响甚微,测定结果在可接受范围内。     

环状扩散采样管的研制及其在大气氨测定中的应用

为解决采样过程中气体与颗粒物之间的相互干扰的问题。在国内首次研制出新型大气痕量气体采样装置－环状扩散管,并应用于采集大气中的氨。在大气条件下对氨的收集效率可达９７％,检测限为０．１５μｇ／ｍ＾３,与滤膜法和湿式环状扩散管进行了对比实验。结果表明三者基本一致,从１９８５年到１９９２年,在４－５月份测定了北京中关村地区大氨浓度,其变化范围４．６－４０μｇ／ｍ＾３,平均浓度１７μｇ／ｍ＾３。     

火焰原子吸收分光光度法测定总铬的研究

用火焰原子吸收分光光度法直接测定水和废水中的总铬.通过不同条件的实验,确定了最佳的分析条件;并通过标准样品和实际样品的分析,验证了方法的准确度和精密度.在大量实验基础上,建立空白实验、准确度质量控制图,以便定期对各种监测数据提供可行的质量保证措施.实验结果表明,该法快速方便,提高了分析效率,准确度高,精密度好,值得普及和推广.     

A new method of simultaneous determination of atmospheric amines in gaseous and particulate phases by gas chromatography-mass spectrometry

As more attention is being paid to the characteristics of atmospheric amines, there is also an increasing demand for reliable detection technologies. Herein, a method was developed for simultaneous detection of atmospheric amines in both gaseous and particulate phases using gas chromatography-mass spectrometry (GC-MS). The amine samples were collected with and without phosphoric acid filters, followed by derivatization with benzenesulfonyl chloride under alkaline condition prior to GC-MS analysis. Furthermore, the method was optimized and validated for determining 14 standard amines. The detection limits ranged from 0.0408-0.421 µg/mL (for gaseous samples) and 0.163-1.69 µg/mL (for particulate samples), respectively. The obtained recoveries ranged from 68.8%-180% and the relative standard deviation was less than 30%, indicating high precision and good reliability of the method. Seven amines were simultaneously detected in gaseous and particulate samples in an industrial park using the developed method successfully. Methylamine, dimethylamine and diethylamine together accounted for 76.7% and 75.6% of particulate and gaseous samples, respectively. By comparing the measured and predicted values of gas-particle partition fractions, it was found that absorption process of aqueous phase played a more important role in the gas-partition of amines than physical adsorption. Moreover, the reaction between unprotonated amines and acid (aq.) in water phase likely promoted water absorption. Higher measured partition fraction of dibutylamine was likely due to the reaction with gaseous HCl. The developed method would help provide a deeper understanding of gas-particle partitioning as well as atmospheric evolution of amines.     

神经网络用于光度法同时测定多种重金属离子

采用可见分光光度法,通过构筑16-5-4多目标神经网络模型实现同时测定溶液中Cd2+、Pb2+、Cu2+、As3+的含量。实验以4-(2-吡啶偶氮)-间苯二酚(PAR)作为显色剂,采用"多因素多水平可视化设计法"设计样本,在4种组分可见吸收光谱严重重叠的390~480 nm范围内,选取16个特征波长处的吸光度作为输入信号,应用"留二法"原则训练BP网络。网络准确预测了结果,Cd2+、Pb2+、Cu2+、As3+的平均回收率分别为100.10%、100.03%、100.09%、99.99%,测定结果的相对标准偏差分别为0.18%、0.12%、0.26%、0.13%,达到了4种组分含量同时测定的目的。