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作 者:侯倩倩 巢静波[2] 许峰 朱天一 张文申 董雅卓 张雨 刘霞 HOU Qianqian;CHAO Jingbo;XU Feng;ZHU Tianyi;ZHANG Wenshen;DONG Yazhuo;ZHANG Yu;LIU Xia(Shandong Nonmetallic Materials Institute,Jinan 250031,China;National Institute of Metrology,Beijing 100013,China)
机构地区:[1]山东非金属材料研究所,济南250031 [2]中国计量科学研究院,北京100013
出 处:《化学分析计量》2023年第9期92-95,共4页Chemical Analysis And Meterage
摘 要:采用高温燃烧吸收仪与离子色谱仪联用技术,建立了测定导电胶中卤素含量的方法。优化的实验条件为:燃烧炉温度为800℃,样品质量为0.1 g,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检测。氯、溴离子质量浓度在1~50 mg/L范围内与对应色谱峰面积线性关系良好,氯离子的线性相关系数r=0.9997,检出限为5.4 mg/kg,加标的平均回收率为101.2%;溴离子线性相关系数r=0.9997,检出限为8.6 mg/kg,加标的平均回收率为100.2%。与传统氧弹燃烧-离子色谱法相比,该法无需对样品进行固化处理,进样方便、快捷,可用于导电胶样品中卤素含量的测定。The method for the determination of chlorine and bromide in conductive adhesive using ion chromatography(IC)with high temperature combustion absorption instruments was established.The optimized conditions were as follows:the temperature of combustion tube were 800℃,the sample weight was 0.1 g,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 mass concentration of chlorine was linear with peak area in the range of 1-50 mg/L,the linear correlation coefficient r=0.9997,the detection limit was 5.4 mg/kg,and the average recoveries were 101.2%.The content of bromide was linear with peak area in the range of 1-50 mg/L,the linear correlation coefficient r=0.9997,the detection limit was 8.6 mg/kg,and the average recoveries were 100.2%.Compared with the traditional oxygen flask combustion-ion chromatography.The method does not need to solidify the sample with convenient and quick sample entry,which can be used for determination of chlorine and bromide in conductive adhesive.
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