徐传军学士学位论文.docVIP

青 岛 科 技 大 学 本 科 毕 业 设 计 （论 文） 题 目 三乙膦酸铝原药全分析 范志先指导教师__________________________ 范志先 辅导教师__________________________ 徐传军学生姓名__________________________ 徐传军 0401010623学生学号__________________________ 0401010623 化工学院（部） 化学工程与工艺 专业 2004级4班 二○○八年六月十八日 中文摘要 PAGE I 三乙膦酸铝原药全分析 摘 要 本文对三乙膦酸铝原药进行了全分析。国产三乙膦酸铝原药中所含杂质主要为亚磷酸盐、硫酸盐和铵盐。对制备的纯品采用离子色谱法定值，含量大于99.0 %，能够满足离子色谱分析对标准品的要求。 本文建立了完整的三乙膦酸铝原药及杂质的离子色谱同时定量分析方法。样品溶解在水中，超声波振荡30 min。采用Na2CO3溶液为淋洗液、AS 9离子色谱柱、电导检测器的定量测定结果表明，方法的准确度（添加回收率100.1 - 100.2 %)和精密度(RSD 0.31 %)均满足常量分析要求，样品测定结果满意。离子色谱法表现出简便、准确、快速、高通量作业的特点。 试验获得了三乙膦酸铝的紫外光谱图、红外光谱图、核磁共振波谱图、质谱图。这些谱图进一步表征了三乙膦酸铝的化学结构。采用离子色谱法，测定的国产三乙膦酸铝原药中除主成分和水分外，大于0.1 %的杂质有亚磷酸根离子、硫酸根离子，铵根离子。亚磷酸根离子、硫酸根离子和铵根离子的含量分别为4.2 - 5.4 %、2.7 - 3.2 %和1.2 - 1.3 %。 关键词：离子色谱法；三乙膦酸铝；农药全分析 ABSTRACT ABSTRACT PAGE II PAGE I THE ANALYSIS OF IMPURITIES FOR FOSETYL-ALUMINUM TECHNICAL ABSTRACT The analysis of impurities for fosetyl-aluminium technical was discussed in this paper. Fosetyl-aluminium technical was made in China, whose impurities are mostly phosphate, sulfate and ammonium. And the prepared pure sample of fosetyl-Al could satisfy the need of ion chromatography analysis. The method of quantitative analysis of fosetyl-aluminium technical and its impurities by ion chromatography with electronic conductivity detector, AS 9 column, Na2CO3 solution as eluent was established. The samples dissolved in the water with ultrasonic oscillating for 30 minutes. The recoveries of two fortification levels were 100.1 - 100.2 % with RSD of 0.31 %. The accuracy and the precision of the method satisfied the need of macro analysis. The result of samples determined was satisfying. The method of ion chromatography is simple, accurate, rapid, and could determine a number of samples simultaneously. The UV spectra, IR spectra, NMR spectrum and mass spectrum of fosetyl-aluminium were obtained in the paper. These spectrograms further characterized the chemical structure of fosetyl-aluminium. All components of fosetyl-aluminium technical made