高等学校化学学报 ›› 2000, Vol. 21 ›› Issue (3): 350.

• 论文 • 上一篇    下一篇

在线固相萃取预富集-原子吸收联用测定痕量Fe(Ⅱ)和总铁量

徐光明, 叶映雪, 殷学锋, 沈宏, Akbar Ali   

  1. 浙江大学化学系, 杭州 310027
  • 收稿日期:1999-07-13 出版日期:2000-03-24 发布日期:2000-03-24
  • 通讯作者: 殷学锋(1945年出生),男,教授,博士生导师,主要从事联用技术和痕量分析研究.
  • 基金资助:

    浙江省自然科学基金资助

Determination of Iron(Ⅱ) and Total Iron Using Flow Injection On line Preconcentration With FAAS

XU Guang-Ming, YE Ying-Xue, YIN Xue-Feng, SHEN Hong, Akbar-Ali   

  1. Department of Chemistry, Zhejiang University, Hangzhou 310027, China
  • Received:1999-07-13 Online:2000-03-24 Published:2000-03-24

摘要: 以1,10-二氮菲(1,10-phen)为配合剂,乙醇为洗脱液,在C18柱上将流动注射固相萃取预富集-原子吸收光谱联用测定痕量Fe(Ⅱ)和总铁.Fe(Ⅲ)的含量可通过抗坏血酸还原后用差示法测得.本法灵敏度高,选择性好,能在线分离干扰富集Fe(Ⅱ),采样速度80次/h,富集倍数19倍,检测下限为3μg/L,相对标准偏差1.1%(n=10),可用于测定水样中痕量Fe(Ⅱ)和Fe(Ⅲ),回收率为94%105%.

关键词: 流动注射, 原子吸收, 在线预富集, Fe(Ⅱ), Fe(Ⅲ)

Abstract: Adirect, rapid and sensitive method for the determination of Fe(Ⅱ) and Fe(Ⅲ) in water samples by flame absorption spectrometry coupled with flow injection on line preconcentration with 1,10-phenanthroline(1,10-phen) as the complex agent was developed. Various parameters affecting the complex formation and its subsequent adsorption, such as pHof the mixture solution, 1,10 phen concentration, sample flow rate etc. were optimized. A 25×10-3 mol/L 1,10 phen in 2.0% ethanol was on line mixed with aqueous sample solution of iron in 0.1%(volume ratio) hydrochloric acid and flowed through the microcolumn for 30 s. Fe(Ⅱ) can be extracted as Fe(Ⅱ)-phen complex in the C18 microcolumn and determined within 10 s in the nebulizer of FAASafter being eluted by ethanol. Ascorbic acid(0.1 mg/mL) was used for the reduction of Fe(Ⅲ) to Fe(Ⅱ). Agood precision(RSD=1.1%, n =10), high enrichment factor(19) and sample throughput(80 h) with detection limit 3 μg/Lwere obtained. The method has been successfully applied on the water sample for Fe(Ⅱ) and Fe(Ⅲ) determination with the recovery 94%—105%.

Key words: Flow injection analysis, Flame atomic absorption spectrometry, On line preconcentration, Fe(Ⅱ),Fe(Ⅲ)

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