流动注射法测定催化剂中.doc

 流动注射在线分离富集-原子吸收法测定催化剂中 痕量钯的研究 摘 要： 以甲醛为交联剂，以三聚氰胺、三乙烯四胺为原料合成了一种新型的三聚氰胺-甲醛-三乙烯四胺（MF-TETA）分离树脂用火焰原子吸收光谱法（FAAS）MF-TETA分离树脂对吸附最佳条件试液中的可被MF-TETA树脂0.16 mol/L硫脲 +0.08 molL HCL混合溶液完全洗脱，洗脱液中的用火焰原子吸收光谱法（FAAS）该法对的检出限为ng/mL (3σ, n = 10)，线性范围为0~6 ug/ml，相关系数r=0.9990，RSD=1.98%，回收率在95.%~99.2%之间三聚氰胺；三乙烯四胺火焰原子吸收光谱法Studies of trace palladium after separation and preconcentration with flow injection system and determination by atomic absorption spectrometry Abstract Melamine-formaldehyde-triethylenetetramine (MF-TETA),a new type of separated resin was synthesized with melamine and triethylenetetramine as raw material and formaldehyde as cross linker. flame atomic absorption spectrometry was the determination method.Flow injection technology was applied to separate and enrich the trace amount of palladium,and then determined the content. This method was to explore the best condition of the separating resin to absorb the palladium. when the pH was 6 and temperature was 20℃,,the palladium in the test solution could be completely absorbed with 2.5 mL/min as the best absorbing rate,and the absorbed palladium can be eluted with the acid thiourea(0.08 mol/L HCL+0.16 mol/L thiourea), and palladium in the eluate could be determined with flame atomic absorption analysis technology.The detection limit of this method was 0.035 ng/mL (3σ, n = 10); The linear range is from 0 to 6 ug/mL,and the correlation coefficient was 0.9990;the coefficient of recovery was between 95.6% and 99.2%. Keywords: melamine;triethylenetetramine;flow injection;flame atomic absorption spectrometry; palladium 目 录 摘 要： 1 第1章 引 言 3 1.1 贵金属的分离方法 3 1.2 流动注射分析法（FIA）简介 3 1.3 螯合吸附树脂简介 3 1.4 立题思想 3 第2章 实 验 部 分 3 2.1仪器和试剂 3 2.1.1 仪器 3 2.1.2 试剂 3 2.2 实验过程 3 2.2.1 PTFE微型柱的制备 3 2.2.2 吸附树脂的制备 3 2.2.3 分析方法 3 2.3结果与讨论 3 2.3.1 酸度对吸附率的影响 3 2.3.2 吸附流速的选择 3 2.3.3 吸附时间的选择 3 2.3.4 洗脱剂的选择 3 2.3.5 洗脱流速的选择 3 2.3.6 工作曲线及检出限 3 2.3.7 共存离子的干扰 3 2.3.8 重复使用实验 3 2.3.9 样品分析 3 2.3.10 吸附原理的探讨 3 参考文献 3 致 谢 3 第1