聚合铝形态的液相色谱分离及其铝元素分析测定方法研究

发布时间：2018-06-17 02:45

本文选题：混凝 + 铝形态　；参考：《河北师范大学》2015年硕士论文

【摘要】：近年来,伴随着全球工业化进程的加速和世界人口的飞速增长,环境问题已成为世界各国人民普遍关注的一个热门话题,尤其面临着水质不断恶化等污染问题。电絮凝已广泛的应用到多种行业的废水处理中。聚合氯化铝(PACl)在水处理中是一种常用到的重要的铝系高分子絮凝剂,聚合氯化铝的研究在水处理行业有重要意义。本硕士学位论文尝试用C18反相高效液相色谱法对PACl混凝剂中铝的不同形态进行色谱分离,并将Ferron逐时络合比色分析与色谱分离相结合进行铝形态的分析测定。对铝的色谱分离条件进行了优化,并分别用石墨炉原子吸收和等离子体质谱法对不同色谱组分中铝的分析测定方法进行了实验研究。主要内容如下:1.对实验室制备的不同碱化度(B值)聚合氯化铝样品,以C18反相高效液相色o}柱进行了不同铝形态的色谱分离,对流动相体系组成和洗脱条件进行了实验优化,并结合Ferron逐时络合比色法对各色谱组分进行了检测分析,得到若干不同铝形态的色谱分离谱图。2.针对聚合铝及其色谱分离后含复杂有机组分基体条件下难原子化元素铝的分析检测问题,以石墨炉原子吸收光谱法进行了实验研究,对热解涂层石墨管进行了涂钽覆膜修饰处理,优化了石墨炉升温程序,建立了针对含有有机溶剂乙腈的PACl样品中铝的分析测定方法,其相对标准偏差RSD=1.74%,检出限为1.54μg/L。3.针对ICP-MS分析具有快速准确,灵敏度高、检测限低等独特优点,在优化HPLC分离条件基础上,对含有有机溶剂乙腈的PACl色谱组分样品中铝的ICP-MS测定方法进行了实验研究,并初步尝试了铝形态的HPLC-ICP-MS联用分析。所建方法线性相关系数达0.9979,加标回收率在98%-103%之间,RSD5%,适合于含有有机物聚合氯化铝溶液中总铝含量的测定。采用优化后石墨炉原子吸收光谱法和ICP-MS方法均检测到色谱传统紫外检测器未检测到的色谱组分。
[Abstract]:In recent years, with the acceleration of the global industrialization process and the rapid growth of the world population, environmental problems have become a hot topic that people all over the world pay close attention to, especially facing the pollution problems such as the deterioration of water quality. Electroflocculation has been widely used in wastewater treatment in many industries. Polyaluminium chloride (PACL) is an important aluminum flocculant in water treatment, and the study of polyaluminium chloride is of great significance in water treatment industry. In this thesis, we try to use C18 reversed phase high performance liquid chromatography to separate the different forms of aluminum in PACl coagulant, and combine Ferron timed complexation colorimetry with chromatographic separation to determine the aluminum speciation. The chromatographic separation conditions of aluminum were optimized and the analytical methods of aluminum in different chromatographic components were studied by graphite furnace atomic absorption spectrometry and plasma mass spectrometry respectively. The main content is as follows: 1. The samples of polyaluminium chloride with different alkalinity (B value) prepared in the laboratory were separated by chromatography with C 18 reversed phase high performance liquid color o} column. The composition of mobile phase system and elution conditions were optimized. The chromatographic components were detected and analyzed by Ferron timed complexation colorimetry, and some chromatographic separation spectra of different aluminum forms were obtained. In view of the problem of the analysis and detection of aluminum, which is difficult to be atomized under the condition of polyaluminium and its chromatographic separation, the graphite furnace atomic absorption spectrometry (GFAAS) has been used to study the analysis and detection of aluminum with complex organic components. The pyrolytic coated graphite tube was modified with tantalum coated film, and the temperature program of graphite furnace was optimized. A method for the determination of aluminum in PACl samples containing organic solvent acetonitrile was established. The relative standard deviation (RSD) was 1.74 and the detection limit was 1.54 渭 g / L. 3. Aiming at the unique advantages of rapid and accurate analysis, high sensitivity and low detection limit, the ICP-MS method for the determination of aluminum in PACl chromatographic samples containing organic solvent acetonitrile was studied on the basis of optimizing the separation conditions of HPLC. The HPLC-ICP-MS analysis of aluminum morphology was also preliminarily attempted. The linear correlation coefficient of the method is 0.9979, and the recovery rate is between 98% and 103%. The method is suitable for the determination of total aluminum in polyaluminium chloride solution containing organic matter. The optimized graphite furnace atomic absorption spectrometry (GFAAS) and ICP-MS method were used to detect the undetectable components in the traditional UV detector.
【学位授予单位】：河北师范大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：O652.63;TQ085.4

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