作者：侯倩倩, 董雅卓, 林帅, 宋磊, 许峰, 张文申, 冀克俭

作者单位：山东非金属材料研究所，山东 济南 250031

关键词：高温燃烧吸收;离子色谱;氟醚橡胶;氟;溴

摘要：

采用高温燃烧吸收仪与离子色谱仪联用技术，建立同时测量氟醚橡胶中氟溴含量的方法。优化的实验条件为：燃烧炉燃烧管进口温度为850 ℃，出口温度为1000 ℃，称样量为10 mg，以0.05 mol/L氢氧化钠为吸收液，0.02 mol/L氢氧化钾为淋洗液，采用抑制型电导检测器。氟离子在1~100 mg/L范围内与其色谱峰面积呈良好的线性关系，线性相关系数r²=0.9993，检出限为0.04%，回收率为93.0%~104.1%。溴离子在0.1~10 mg/L范围内与其色谱峰面积呈良好的线性关系，线性相关系数r²=0.9996，检出限为0.005%，回收率为94.0%~104.0%。与传统氧瓶燃烧、氧弹燃烧-离子色谱法相比，该方法方便、快捷，可连续处理样品，在30 min之内即可完成样品的检测。

Determination of fluorine and bromine in fluoroether rubber by high temperature combustion absorption-ion chromatography
HOU Qianqian, DONG Yazhuo, LIN Shuai, SONG Lei, XU Feng, ZHANG Wenshen, JI Kejian
Shandong Nonmetallic Materials Institute, Jinan 250031, China
Abstract: The method for the determination of fluorine and bromine in fluoroether rubber using ion chromatography (IC) with high temperature combustion absorption instruments was established. The optimized conditions were as follows: the inlet temperature and outlet temperature of combustion tube were 850 ℃ and 1000 ℃, the sample weight was 10 mg, and 0.05 mol/L NaOH solution was used as absorbent. 0.02 mol/L KOH solution was used as eluant, and restraining conductance detector was used in determination. The content of fluorine was linear with peak area in the range of 1-100 mg/L, the linear correlation coefficient r²=0.9993, the detection limit was 0.04%, and the recoveries are between 93.0%-104.1%. The content of bromide was linear with peak area in the range of 0.1-10 mg/L, the linear correlation coefficient r²=0.9996, the detection limit was 0.005%, and the recoveries are between 94.0%-104.0%. Compared with the traditional oxygen flask combustion-ion chromatography, this method is accurate and fast. It can process the sample continuously and complete the sample detection within 30 minutes.
Keywords: high temperature combustion absorption;IC;fluoroether rubber;fluorine;bromine
2020, 46(8):53-58  收稿日期: 2020-03-12;收到修改稿日期: 2020-04-20
基金项目: 国防科工局技术基础项目（JSJL2017208A013）
作者简介: 侯倩倩（1985-），女，山东潍坊市人，副研究员，博士，主要从事化学分析与计量工作
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