Determination of trace triethylamine in polycarbonate polymerization solution by headspace-gas chromatography
PANG Yuna, GONG Bin, FENG Qingxia, HU Changying, YANG Shuo
Luxi Chemical Industry Group Co., Ltd., Liaocheng 252000, China
摘要：建立顶空-气相色谱法测定聚碳酸酯聚合溶液中三乙胺含量的快速测定方法。用乙醇将聚合溶液中的聚碳酸酯沉淀，滤液以二氯甲烷 、乙醇 、10%（质量分数）氢氧化钠溶液混合溶剂溶解定容，采用顶空-气相色谱法检测，色谱峰面积外标法定量。以 DB-624 柱（30 m×0.25 mm×1.4 μm）为分离柱；载气为氮气，流量为 1.2 mL/min；柱温升温程序：初始温度为 80 ℃，以 10 ℃/min 的升温速率升至 220 ℃；进样口温度为 200 ℃；FID 检测器温度为 250 ℃；进样体积为 0.6 mL；采用分流进样，分流比为 20∶1。三乙胺质量浓度在 0.2～2.0 mg/L 范围内与色谱峰面积线性相关，相关系数为 0.999 5，方法检出限为 0.12 mg/L。 样品加标回收率为 98.47%～100.05%，测定结果的相对标准偏差为 0.42%～1.34%（n=6）。该方法操作简单，适用于工业生产聚碳酸酯聚合溶液中三乙胺的批量快速检测。
Abstract：A method of rapid determination of trace triethylamine in polycarbonate polymerization solution by headspace-gas chromatography was established. The polycarbonate in the polymeric solution was precipitated with ethanol, and the mixture of methylene chloride, ethanol and 10% (mass fraction) sodium hydroxide solution was filled with a constant volume. Then, headspace-gas chromatography was used for detection and external standard method for chromatographic peak area was used for quantification. Chromatographic experiments conditions were as the following: DB-624 column (30 m ×0.25 mm ×1.4 μm) was used as separation column; the nitrogen was used as carrier gas with the flow rate of 1.2 mL/min; the column temperature was programmed: the initial column temperature was 80 ℃, then the column temperature was raised to 220 ℃ at the heating rate of 10 ℃/min; the inlet temperature was 200 ℃; the FID detector temperature was 250 ℃; the injection volume was 0.6 mL; split injection with the split ratio of 20∶ 1. The mass concentration of triethylamine had a good linear relationship with the chromatographic peak area in the range of 0.2-2.0 mg/L, the correlation coefficient was 0.999 5, and the detection limit of the method was 0.12 mg/L. The recovery of sample spiking was 98.47%-100.05%, and the relative standard deviation of the determination results was 0.42%-1.34% (n=6). The method has the advantages of simple operation, and it is suitable for batch rapid detection of triethylamine in dustrial production of polycarbonate polymerization solution.
Keywords：headspace-gas chromatography; polycarbonate; polymerization solution; triethylamine
PANG Yuna，GONG Bin，FENG Qingxia，et al. Determination of trace triethylamine in polycarbonate polymerization solution byheadspace-gas chromatography[J]. Chemical Analysis and Meterage，2023，32(10)：62.