【摘要】 报告了毛细管气相色谱 原子吸收联用技术研究中对卧管式微火焰原子化离子化同步检测器性能的改进和零死体积传输线的研究成果。在已有研究基础上 ,对卧管式微火焰原子化离子化同步检测器T型玻璃管及卧式长管不锈钢收集极的物理尺寸及相关操作条件进行了最佳化研究 ,同时 ,在T型玻璃管两端安装了石英玻璃窗 ,稳定了管内气流 ,改善了敏感度。二乙基汞原子化敏感度为 1 .4× 1 0 - 1 2 g s,线性范围 4 .2× 1 0 2 ,峰面积重现性 (RSD) 1 .7% ;苯离子化敏感度为 3 .5× 1 0 - 1 1 g s,线性范围 4 .0× 1 0 5,峰面积重现性 (RSD) 1 .5 %。研制了自动控温零死体积传输线 ,基本消除了由于传输线死体积中分子扩散导致的分辨率损失 ,顺利实现了毛细管色谱柱与卧管式微火焰原子化离子化同步检测器的连接。更多还原

【Abstract】 Gas chromatography/atomic absorption spectroscopy (GC/AAS) is a good method for the species analysis of organometallic compounds. But the traditional atomizers are not very suitable for the technology and all of them response only to one kind of signal--the concentration of the metallic atoms of the ground state. They can not give any information about the organic component of organometallic compounds or coexisteol organic compounds. Therefore, we had designed and manufactured a new type detector that can sensitively and synchronously response to the atomization signal of organometallic compound and ionization signal of organic compound. On this basis, we introduced capillary column to GC/AAS technology and designed and manufactured a zero dead volume transfer line. The molecular diffusion within the transfer line has been removed almost completely. So the resolution loss was almost zero. Meanwhile, we improved the character of the horizontal pipe mini-flame atomization and ionization synchronous detector. Sizes of the T type glass tube and long pipe stainless steel collector of horizontal pipe mini-flame atomization and ionization synchronous detector have been optimized, and the quartz windows have been fixed on both ends of the T type glass tube. This can decrease the noise and stabilize the output of signal. The detection limit of atomization for the organometallic compound (diethylmercury) is 2.3×10 -12 g/s and of ionization for the organic compound (benzene) is 3.5×10 -11 g/s. The linear range is 4.2×10 2 for atomization of diethylmercury ( r =0.9997) and 4.0×10 5 for ionization of benzene ( r =0.9996). The relative standard deviation (RSD, n =11) of the peak area in the optimum operating condition of atomization for the organometallic compound (diethylmercury) and of ionization for the organic compound (benzene) is 1.8% and 1.5% respectively.更多还原