微库仑法测定多种有机液体化工产品中的氯含量

Determination of total chlorine in organic chemical products by microcoulometry

建立了测定多种有机液体化工产品中氯含量的微库仑法;通过实验,优化了裂解炉温度、氩气（载气）流量、二次燃烧时氧气流量、二次燃烧时间、液体进样速度等分析条件;考察了该方法的准确度和重复性,并确定了方法的最低检出限。实验结果表明,微库仑法适宜的分析条件为：裂解炉温度1050℃、氩气流量150mL/min、二次燃烧时氧气流量100mL/min、二次燃烧时间为60s、液体进样速度0.5μL/s。采用微库仑法分析有机液体化工产品中的微量氯,回收率在90.6%～109.4%之间;试样重复测定3次的相对标准偏差在0.10%～2.87%之间,氯的最低检出限在0.17mg/L。该方法准确可靠,检测范围宽,可满足多种有机液体化工产品中氯含量测定的需要。

A method for determination of total chloride content in organic chemical products was established by microcoulometry.The experimental results showed that under the optimal conditions of combustion oven temperature 1050℃,the flow rate of argon was 150mL/min,the flow rate of oxygen in the 2nd combustion was 100mL/min,the 2nd combustion time was 60 sand the sample injection rate was 0.5μL/s.The average recoveries of total chlorine in organic chemical products were between 90.6%-109.4%.The RSDs were between 0.10%-2.87%.The detection limit of total chloride in organic chemical products was 0.17mg/L.The method is simple,rapid,sensitive and suitable for trace total chloride analysis in organic chemical products.