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

doi:10.3724/SP.J.1123.2016.10002

Abstract

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

CLC Number:

O658

NI Lijun, LIU Jianyun, CHEN Zhu, TANG Bingjing, WANG Fang, LUAN Shaorong. Determination of trace chlorine in caprolactam by ion chromatography coupled with multiple pyrolysis and enrichment pretreatment[J]. Chinese Journal of Chromatography, 2017, 35(3): 314-317.

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