高等学校化学学报

高等学校化学学报 ›› 1994, Vol. 15 ›› Issue (12): 1766.

• 论文 • 上一篇    下一篇

流动注射预富集─石墨炉原子吸收联用测定海水中痕量钼

殷学锋, 刘梅   

  1. 浙江大学化学系, 杭州, 310027
  • 收稿日期:1994-01-12 修回日期:1994-05-07 出版日期:1994-12-24 发布日期:1994-12-24
  • 通讯作者: 殷学锋.男,49岁,副教授.
  • 作者简介:殷学锋.男,49岁,副教授.
  • 基金资助:

    国家自然科学基金

Determination of Ultfa-trace Amounts of Molybdenum in Seawater by Flow Injection On-line Preconcentration Graphite Furnace Atomic Absorption Spectrometry

YIN Xue-Feng, LIU Mei   

  1. Department of Chemistry, Zhejiang University, Hangzhou, 310027
  • Received:1994-01-12 Revised:1994-05-07 Online:1994-12-24 Published:1994-12-24

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摘要： 用二乙基二硫代氨基甲酸钠作络合剂、乙醇作洗脱液的流动注射固相吸附萃取预富集─石墨炉原子吸收联用测定海水中痕量钼。设计了以固定体积取样法为基础的预富集装置。考察了实验参数对分析性能的影响。本法能在线分离干扰、富集被测物,当样品上柱体积为1.35mL时,富集倍数为13.3倍,检测下限为0.027μg/L,用于测定海水等标样中钼含量,精密度较好。

关键词: 流动注射, 固相萃取, 原子吸收分光光度法, 预富集, 钼

Abstract: Amethod for determination of ultra-trace amounts of molybdenum in seawater by flow injection on-line sorbent extraction preconcentration coupled with GFAASis described.An approach for introducting only the most concentrated fraction of the eluate into the graphite tube while discarding the rest was investigated. The experimental parameters of the FI-GFAASwere optimized. If miniflow (50 mL/min) in atomisation step was used, the memory effect in the determination of molybdenum by graphite furnace could be removed. By using the preheating step in furnace temperature program, diffusion losses of molybdnum ethanol solution could be prevented. On-line chelation of molybdenum with dithiocarbamate (NaDDTC) and sorption of the complex on C18 sorbent packed in a micro column ensure high group selectivity and enrichment. The closed nature of flow system reduced the risk of contamination significantly. The enrichment factor was 13. 3 using sample loading volume of only 1. 35 mL, detection limit achieved was 0.027μg/L. Results obtained for seawater and riverwater standards agreed well with certified values with a good precision.

Key words: Flow-Injection, Sorbent extraction, GFAAS, Preconcentration, Molybdenum

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