摘要
利用气相色谱反吹技术,针对二氨基二苯甲烷产品的高沸点、多组分、粘度大的特点,采用氢火焰检测器;安装六通阀、锥形阀、电磁阀,实现气路转换、气路平衡、气路反吹功能;筛选多种色谱柱,调节进样口温度、柱箱温度、反吹时间等:选用SE-30填充柱(3 m×3 mm),进样口温度280℃,检测器温度280℃,柱箱温度100℃(1 min)-40℃/min-120℃(0.1 min)-60℃/min-260℃(4 min),在2.8 min开启反吹,反吹时间3.6 min。苯胺含量在0.096~3.110 mg/m L之间呈良好线性关系,相关系数为0.9916,检出限为13.04μg/m L,样品加标回收率在93.5%~106.3%之间,RSD小于4.4%.实验验证反吹气路和分析方法的可行性,方法适用于工业分析。
In order to analyze 4,4＇-diaminodiphenyl methane, which has high boiling point, multi component and high viscosity, the technology of gas chromatography counter blowing and FID detector were performed. The six way valve, cone valve and electronic valve were installed to realize the function of transformation, balance and reverse blow of the gas path. The temperature of the injection, the oven and the time of reverse blow were adjusted through filtrating various types of chromatographic columns. The results showed that the SE -30 column（3m × 3mm）was adopted, and the temperature of the injection and the detection were set at 280℃, respectively. The process of oven was from 100℃ （1 min）to 120℃ （0. 1 min） （the flow was 40℃/ min） and then arrived at 260℃ （4 min） （the flow was 60℃/min）, and reverse blow started at 2.8 min to keep blowing for 3.6 min. The good linear relationship was showed between 0. 096 - 3.110 mg/mL of aniline with the correlation coefficient of 0. 9916, the detection limit of 13.04 μg/mL, and the recovery rate between 93.5% -106. 3%. The precision was less than 4. 4%. The experiments verified that the analysis of gas path of reverse blow was feasibl and this method is simple, fast and accurate. It was applied to industrial analysis.
出处
《分析试验室》
CAS
CSCD
北大核心
2017年第1期92-95,共4页
Chinese Journal of Analysis Laboratory
关键词
气相色谱
反吹法
苯胺
二氨基二苯甲烷
Gas chromatography
Reverse blow
Aniline
4,4＇-DiaMinodiphenylMethane
