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在气相色谱分析中,有关程序涂渍色谱柱的研究已有报道,这种色谱柱较适合于厚涂柱的分析。本文所研制的指数程序薄涂色谱柱及分析应用,尚未见报道。该色谱柱是将一根色谱柱分成几段,将每段的固定液涂渍量按指数函数y=m~i(i=1,2,3)变化,而每段固定液量都不超过1％,色谱柱选定为1m。由于固定液量少,且采用指数程序涂渍,因此,色谱操作柱温可较低,分离效能较高,组分的保留时间短,很适合较高沸点、易分解化合物的直接快速分析。 此色谱柱应用于实际样品中己二酸(沸点为330℃,近沸点时分解)的分析,己二酸于160℃下出峰快,保留时间短,峰形较对称,容易定量。其最小检测量为0.80μg,回收率为101.5％,相对标准偏差为±5.9％。 实验部分 (一)主要仪器与色谱条件 1.仪器 上海103气相色谱仪,热导池检测器,岛津C-R3A数据处理机。 2.色谱条件 色谱柱为1m×0.3mm不锈钢柱;固定液为QF-1按0.34％、0.49％、0.7％涂渍;载体为硅烷化玻璃微球(80～100目);载气(H_2)流速40ml/min;桥流150mA;汽化温度172℃;柱温160℃;检测温度170℃。 (二)试剂
In gas chromatographic analysis, there have been reports of procedure-coated columns that are more suitable for thick-coated columns. The index program developed in this paper thin coating chromatography column and analysis and application, has not been reported. The column is a column is divided into several sections, each section of the fixed liquid coating amount according to the exponential function y = m ~ i (i = 1,2,3) change, and each fixed amount of fluid does not exceed 1%, the column is selected as 1m. Due to the low fixed volume and the application of exponential program, the chromatographic column temperature can be lower, the separation efficiency is higher, the retention time of the components is short, and it is suitable for direct and rapid analysis of higher boiling and easily decomposing compounds. This column is used in the actual sample adipic acid (boiling point of 330 ° C, decomposition near the boiling point) analysis, adipic acid peak at 160 ° C fast, short retention time, the peak shape is more symmetrical, easy to quantify. The minimum detectable amount was 0.80μg, the recovery was 101.5% and the relative standard deviation was ± 5.9%. Experimental part (A) of the main instruments and chromatographic conditions 1. Instrument Shanghai 103 gas chromatograph, thermal conductivity detector, Shimadzu C-R3A data processor. 2. Column chromatography conditions 1m × 0.3mm stainless steel column; fixed solution QF-1 by 0.34%, 0.49%, 0.7% coating; silanized glass microspheres (80 ~ 100 mesh); carrier gas ) Flow rate 40ml / min; bridge flow 150mA; vaporization temperature 172 ℃; column temperature 160 ℃; detection temperature 170 ℃. (B) Reagents