在线燃烧离子色谱法测定环氧树脂中的氯和溴

Determination of chlorine and bromine in epoxy resins by online combustion ion chromatography

建立了在线燃烧离子色谱同时测定环氧树脂中氯和溴的分析方法.采用高温裂解炉与离子色谱的在线联用装置,通过对样品进行高温燃烧裂解和气化,以100 mg·L^(-1)过氧化氢为吸收液,将产生的卤化氢气体吸收并转化为无机阴离子,离子色谱法进行样品的测定,以氯和溴的峰面积外标法进行定量.对影响燃烧效果和测定结果准确度的因素如燃烧时间、燃烧温度、吸收液体积、称样量、氧气和氩气流速等条件进行了选择优化.在(0.10—2.50)mg·L^(-1)和(0.02—0.50)mg·L^(-1)范围内,氯和溴离子的线性相关系数(r^(2))大于0.999,该方法对于氯和溴的定量下限分别为0.55 mg·kg^(-1)和2.60 mg·kg^(-1).采用建立的方法分别对环氧树脂和EC680k低密度聚乙烯标准物质中的氯和溴进行测定,并与传统的氧弹燃烧-离子色谱法进行了比较.结果表明:在线燃烧离子色谱法对于环氧树脂中氯和溴测定结果的相对标准偏差分别为1.28%和2.29%,测定值与氧弹燃烧-离子色谱法基本一致,EC680k的测定结果与标准值符合,证明该方法具有良好的准确度和精密度.该方法准确度和灵敏度高、重复性较好,能够满足批量树脂类样品中氯和溴的含量筛查和多批次产品的质量控制.

A method for the simultaneous determination of chlorine and bromine in epoxy resins by online combustion ion chromatography was developed.High-temperature pyrolysis furnace coupled with ion chromatography was used to decompose and gasify the samples at high temperature,and hydrogen peroxide(100 mg·L^(-1))was used as absorbent.The resulting hydrogen halide gas was absorbed and transformed into inorganic halogen anions,and the samples were separated and determined by ion chromatography,which was quantified by an external standard method using the peak area of chlorine and bromine.Parameters that affect the combustion effect and the accuracy of the results such as combustion time,combustion temperature,the volume of the absorption liquid,sample weight,and the flow rate of oxygen and argon were optimized.In the range of(0.10—2.50)mg·L^(-1) and(0.02—0.50)mg·L^(-1),the linear correlation coefficient(r^(2))of chlorine and bromine was greater than 0.999.The limits of quantitation of this method for chlorine and bromine was 0.55 mg·kg^(-1) and 2.60 mg·kg^(-1),respectively.Chlorine and bromine in epoxy resins and EC680k low-density polyethylene certified reference materials were determined by the established method,and the results were compared with the traditional oxygen bomb combustion-ion chromatography.The results showed that the relative standard deviations of chlorine and bromine in epoxy resins were 1.28%and 2.29%,respectively,which were consistent with the results of oxygen bomb combustion-ion chromatography,the determination results of EC680k wee in accordance with the certified value,which proves that the method has good accuracy and precision.The method has high accuracy,sensitivity and repeatability,and can meet the requirements of screening chlorine and bromine content in batch samples and quality control of multi-batch products.