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离子色谱法测定碳酸盐及磷酸盐中四种无机阴离子

韩婷婷,崔 鹤,段小娟,宋 田,姬泓巍,李慧新,蔡 峰,朱倩林   

  1. 1.中国海洋大学化学化工学院,山东 青岛 266100;2.山东出入境检验检疫局检验检疫技术中心,山东 青岛 266002;
    3.青岛出入境检验检疫局,山东 青岛 266001;4.燕山大学理学院,河北 秦皇岛 066004
  • 出版日期:2016-07-25 发布日期:2016-07-26
  • 通讯作者: 崔 鹤
  • 基金资助:

    国家重大科学仪器设备开发专项(2012YQ090229)

Determination of Four Inorganic Anions in Carbonates and Phosphates by Ion Chromatography

HAN Tingting, CUI He, DUAN Xiaojuan, SONG Tian, JI Hongwei, LI Huixin, CAI Feng, ZHU Qianlin   

  1. 1. College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266100, China;
    2. Shandong Entry-Exit Inspection and Quarantine Technology Center, Qingdao 266002, China;
    3. Qingdao Entry-Exit Inspection and Quarantine Bureau, Qingdao 266001, China;
    4. College of Science, Yanshan University, Qinhuangdao 066004, China
  • Online:2016-07-25 Published:2016-07-26
  • Contact: CUI He

摘要:

建立离子色谱等度分离测定碳酸盐及磷酸盐中F-、Cl-、SO42-、NO3- 4 种无机阴离子的方法,碳酸盐试样用20 mmol/L氢氧化钠溶液溶解,加磷酸中和至pH 4.5~5.5;磷酸盐试样直接用20 mmol/L氢氧化钠溶液溶解。色谱柱采用AS11-HC分离柱,流动相20 mmol/L氢氧化钠溶液,流速1.0 mL/min。结果表明:F-、Cl-、SO42-、NO3-4 种阴离子质量浓度与峰面积呈良好线性关系(r = 0.999 2~0.999 9),检出限分别为2.0、2.0、2.5、2.5 mg/kg,在低、中、高3 个加标水平下的平均回收率为80%~109.88%,相对标准偏差为0.85%~4.67%(n=6)。该方法准确、简便、灵敏、通用、重复性好,可用于碳酸盐及磷酸盐中4 种阴离子的实际检测。

关键词: 离子色谱法, 碳酸盐, 磷酸盐, 无机阴离子

Abstract:

An analytical method using ion chromatography with isocratic elution was developed for the determination of four
inorganic anions (F-, Cl-, SO42-  and NO3-) in carbonates and phosphates. Carbonate samples were dissolved in 20 mmol/L
sodium hydroxide solution and then neutralized to pH between 4.5 and 5.5 with phosphoric acid. Phosphate samples were
dissolved with 20 mmol/L sodium hydroxide solution directly and then separated on an AS11-HC column with 20 mmol/L
sodium hydroxide solution as the mobile phase at 1.0 mL/min flow rate. The results indicated that the calibration curves
showed good linear relationship for 4 inorganic anions (r = 0.999 2–0.999 9). The limits of detection (LODs) for F-, Cl-,
SO42- and NO3- were 2.0, 2.0, 2.5 and 2.5 mg/kg respectively. The mean recoveries at three spiked concentration levels
(low, middle, and high) were 80%–109.88%, and the relative standard derivations (RSDs) were 0.85%–4.67% (n = 6).
The proposed method is reliable, simple, convenient, sensitive, universal and reproducible, and can be applied in the rapid
determination of 4 anions in carbonates and phosphates.

Key words: ion chromatography, carbonate, phosphate, inorganic anion

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