色谱

色谱 ›› 2017, Vol. 35 ›› Issue (3): 314-317.DOI: 10.3724/SP.J.1123.2016.10002

• 研究论文 • 上一篇    下一篇

多次高温裂解、富集-离子色谱法检测己内酰胺中的痕量氯

倪力军, 刘建云, 陈筑, 唐冰静, 王芳, 栾绍嵘   

  1. 华东理工大学化学与分子工程学院, 上海 200237
  • 收稿日期:2016-10-05 出版日期:2017-03-08 发布日期:2013-07-16
  • 通讯作者: 栾绍嵘,Tel:(021)64252832,E-mail:srluan@ecust.edu.cn.
  • 基金资助:

    华东理工大学煤气化及能源化工教育部重点实验室开放基金（2016KY11-042）.

Determination of trace chlorine in caprolactam by ion chromatography coupled with multiple pyrolysis and enrichment pretreatment

NI Lijun, LIU Jianyun, CHEN Zhu, TANG Bingjing, WANG Fang, LUAN Shaorong   

  1. School of Chemistry & Molecular Engineering, East China University of Science & Technology, Shanghai 200237, China
  • Received:2016-10-05 Online:2017-03-08 Published:2013-07-16
  • Supported by:

    Open Fund from Key Laboratory of Coal Gasification and Energy Chemical Engineering of Ministry of Education of East China University of Science and Technology (No. 2016KY11-042).

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摘要：

建立了多次高温裂解、富集-离子色谱检测己内酰胺（CPL）中痕量氯的分析方法。CPL样品在富氧环境下经3次高温（800 ℃）裂解后，痕量有机氯转化为氯气或氯化氢气体，经5 mL 10 mmol/L的NaOH溶液吸收、富集，然后转化为氯离子，在阴离子抑制电导检测模式下进行离子色谱分析，检测其中氯离子（Cl-）的含量。在优化的条件下，Cl-在0.05~1.0 mg/L范围内呈良好线性，相关系数为0.9997，方法检出限为0.37 μg/g。对0.8 mg/L的Cl-标准溶液连续进样7次，其保留时间、峰面积、峰高的RSD分别为0.04%、0.24%和0.20%；分别对CPL样品进行处理和检测，得到痕量氯含量的RSD为1.52%（n=4）；Cl-标准溶液的转化率为93.3%~104.0%，CPL样品的加标回收率为95.3%~113.1%。该方法操作简单、前处理条件可控、重复性好、检出限低，可满足实际样品中痕量氯的检测。

关键词: 多次高温裂解与富集, 痕量氯, 己内酰胺, 离子色谱

Abstract:

A method was developed for determination of trace chlorine in caprolactam samples by ion chromatography (IC) coupled with multiple pyrolysis and enrichment pretreatment. The caprolactam samples were treated by multiple pyrolysis at 800℃. Trace organic chlorine in samples was decomposed into chlorine or hydrogen chloride. The gas products of pyrolysis were absorbed and enriched in 5 mL 10 mmol/L NaOH solution, which was analyzed by IC with suppressed conductor. Under the optimum conditions, the linear relationship of Cl- was good in the range of 0.05-1.0 mg/L with correlation coefficient of 0.9997. The method detection limit of chlorine in caprolatam samples was 0.37 μg/g. For 0.8 mg/L Cl- standard solution, the RSDs of retention time, peak area and peak height were 0.04%, 0.24%, and 0.20%, respectively (n=7). The RSD of the contents of chlorine in caprolactam samples was 1.52% (n=4). The conversion ratio of Cl- standard solution ranged from 93.3% to 104.0%, and the spiked recoveries of the samples ranged from 95.3% to 113.1%. The method was applied to determine the contents of chlorine in caprolactam samples with simple operation, controlled pretreatment, low blank, low detection limit, good reproducibility and satisfactory results.

Key words: caprolactam, ion chromatography (IC), multiple pyrolysis and enrichment pretreatment, trace chlorine

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