气相色谱法测定分子筛生产循环废水中的三乙胺及杂质含量

采用气相色谱-质谱仪对晶化母液处理回收工艺流程中的三乙胺及杂质含量进行了定性分析,确定了三乙胺的杂质种类,为建立气相色谱分析方法确立了目标组分。在筛选色谱柱和优化色谱条件的基础上,选用十六烷醇柱CP7448(0.32 mm×60 m×0.5μm),TCD检测器,测定回用三乙胺产品的纯度和杂质含量,实验结果表明,目标组分分离效果良好。以校正面积归一法对三乙胺及杂质的质量分数进行定量,各组分重复测定5次的相对标准偏差均小于1.8%,回收率在98.5%~103.0%之间,表明方法的精密度和准确度良好,并具有快速、可靠的特点。

Determination of triethylamine and impurities in recycling wastewater of molecular sieve production by gas chromatography

Abstract：The content of triethylamine and impurities in crystallized mother liquid recycling wastewater is quantitatively analyzed by means of GC-MS. The impurities in determined and the target components are established for setting up GC method. Based on the optimal chromatographic conditions, the capillary column CP7448（ φ0. 32 mm×60 m×0. 5 um） is chosen as chromatographic column, the purity of recycling triethylamine and the content of impurities are determined using TCD detector. The resuhs show that the target components can be well separated and analyzed. The calibration area normalization method is used to calculate the mass fraction of tri- ethylamine and impurities, the RSD of five times repeated analysis is within 1.8% and recovery rate is from 98. 5% to 103.0%, which indicates good precision and accuracy, and has advantages of rapid and reliable.