色谱2017，Vol.35Issue(3)：314-317,4.DOI:10.3724/SP.J.1123.2016.10002
多次高温裂解、富集-离子色谱法检测己内酰胺中的痕量氯
Determination of trace chlorine in caprolactam by ion chromatography coupled with multiple pyrolysis and enrichment pretreatment
摘要
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 0.999 7.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.关键词
离子色谱/多次高温裂解与富集/己内酰胺/痕量氯Key words
ion chromatography (IC)/multiple pyrolysis and enrichment pretreatment/caprolactam/trace chlorine分类
化学化工引用本文复制引用
倪力军,刘建云,陈筑,唐冰静,王芳,栾绍嵘..多次高温裂解、富集-离子色谱法检测己内酰胺中的痕量氯[J].色谱,2017,35(3):314-317,4.基金项目
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).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). （2016KY11-042）
