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    离子色谱法直接测定聚合级乙二醇中痕量氯离子

    Direct Determination of Trace Chloride Ion in Polymeric Grade Ethylene Glycol by Ion Chromatography

      摘要
    • 摘要: 分别采用KOH和Na2CO3/NaHCO3淋洗液体系，建立了离子色谱直接测定聚合级乙二醇中痕量氯离子含量的两种方法。采用抽真空手动进样方式，分别以IonPac AS19（4 mm×250 mm）为分析柱，IonPac AG19（4 mm×50 mm）为保护柱，5 mmol·L-1 KOH溶液为淋洗液；以IonPac AS23（4 mm×250 mm）为分析柱，IonPac AG23（4 mm×50 mm）为保护柱，4.5 mmol·L-1 Na2CO3-0.8 mmol·L-1 NaHCO3混合溶液为淋洗液进行分离，以电导检测器检测。两种方法中，氯离子的质量比在一定范围内与峰面积呈线性关系，检出限（10S/N）分别为0.002，0.006 mg·kg-1，加标回收率分别为94.7%~100%，92.3%~99.8%，测定值的相对标准偏差（n=3）小于5.0%。两种方法测定聚合级乙二醇中痕量氯离子的结果具有一致性。

       

      Abstract: With KOH solution and Na2CO3/NaHCO3 solution as eluents, two methods were developed for the direct determination of trace chloride ion in polymeric grade ethylene glycol (EG) by ion chromatography, respectively. Vacuum manual sample introduction mode was used. Chloride ion in the sample was seperated on IonPac AS19 analytical column (4 mm×250 mm) and IonPac AG19 guard column (4 mm×50 mm) with 5 mmol·L-1 KOH solution for elution, or on IonPac AS23 analytical column and IonPac AG23 guard column (4 mm×50 mm) with 4.5 mmol·L-1 Na2CO3-0.8 mmol·L-1 NaHCO3 solution for elution, and detected by conductivity detector. In the two methods, linear ralationships were found between the peak area and the mass ratio of chloride ion in definite ranges, with detection limits (10S/N) of 0.002, 0.006 mg·kg-1, respectively. Recovery rates obtained by standard addition method were 94.7%-100%, 92.3%-99.8%, respectivly, and RSDs (n=3) were both less than 5.0%. The determination results of trace chloride ion in polymeric grade ethylene glycol by the two methods were consistent.

       

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