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建立了一种新的二维离子色谱分析模式,应用阀切换技术并联抑制电导和脉冲安培双检测体系,同时测定Cl-、NO-2、SO2-4、NO-3和葡萄糖酸根离子。第一维色谱采用 Ionpac AG18+Ionpac AS18阴离子分析柱,分别以5和20 mmol/L的 NaOH溶液等度淋洗,流速为1.0 mL/min,进样量为25μL,抑制电导检测 Cl-、NO-2、SO2-4和 NO-3。第二维色谱采用 CarboPac PA1+CarboPac PA20两保护柱串联,以90 mmol/L NaOH溶液、0.8 mL/min的流速洗脱,由 AG15柱分离富集葡萄糖酸根,脉冲安培检测器检测。结果表明:无机阴离子在0.1~5.0 mg/L、葡萄糖酸根在0.0856~4.2825 mg/L范围内有良好的线性关系,RSD 在1.05%~1.94%之间,相关系数(R2)在0.9945以上;无机阴离子的方法检出限为0.615~2.17μg/L,葡萄糖酸根的方法检出限为24.24μg/L;回收率在90.3%~102.8%之间。该方法并联两种检测模式,有良好的准确度和精密度,适用于复杂样品的分离分析。

A new two-dimensional ion chromatography method was developed to parallelly analyze two different types of samples with the application of valve switching technology-sup-pressed conductivity and pulsed amperometric analysis system ,for concurrent determination of chloride,nitrite,sulfate,nitrate four inorganic anions and gluconate. The first dimensional chromatography was using Ionpac AG18+Ionpac AS18 anion analysis columns with a suppressed conductivity detector for the separation and detection of Cl-, NO-2 , SO 2-4 and NO-3 . Respectively,the elution was 5 and 20 mmol/L NaOH at an isocratic flow rate of 1. 0 mL/min and sample injection volume of 25 μL. The second dimensional chromatography was utilizing two guard columns,CarboPac PA1 and CarboPac PA20,with 90 mmol/L NaOH solution for the isocratic eluent of 0. 8 mL/min. Gluconate was enriched by an AG15 column and switched into the pulsed amperometric detector. The results showed that:each inorganic anion in 0. 1-5. 0 mg/L and gluconate in 0. 085 6-4. 282 5 mg/L had a good linear relationship(R2≥0. 994 5). The RSDs of the peak areas were between 1. 05%-1. 94%. The limits of detection were 0. 61-2. 17μg/L for the anions and 24. 24 μg/L for the gluconate. The recoveries were between 90. 3%-102. 8%. The two detection modes parallelly have good separation efficiency,detection accura-cy and the precision of the separation and are suitable for the analysis of complex samples.

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