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ICP-MS测量超痕量钚时质谱干扰的消除及水中钚的测定
Elimination of Spectral Interferences for ICP-MS and Determination of 239Pu in Water
【摘要】 研究了感应耦合等离子体质谱(ICP MS)测定超痕量钚时的质谱干扰及干扰元素的去除;建立了环境水样中超痕量钚的测定方法。方法所用的解吸液适于ICP MS直接进样,并有效地消除铅等元素形成的多原子离子干扰。测量了溶液中的m/z238和2%HNO3空白液中的239Pu和242Pu计数率,对测量结果进行校正。方法的本底为20fg,方法对239Pu的检出限为43fg,测定限为88fg。所分析的水样中,井水中的239Pu含量低于检出限,地表水中239Pu的含量高于检出限,湖水和河水中的239Pu高于测定限,但属于全球沉降引起的本底,不会对公众造成辐射危害。
【Abstract】 The spectral interferences derived from metal U,Pb,Hg and Tl,may occur when ICP-MS is used to determine ultratrace plutonium,but, which could be eliminated by the separation procedure using anion exchange resin.The plutonium in water is isolated with Fe(OH)3 (coprecipitation),followed by purification using anion exchange resin with employing nitric acid and hydrochloric acid to rinse above mentioned ions. The eluate,0.01 mol/L HNO3-0.01 mol/L HF,can be introduced directly to the sample injector,and is beneficial for the elimination of polyatomic PbCl+. The concentration of 239Pu in water is measured by isotope dilution using 242Pu as the spike after the reported (ratio,)239Pu/242Pu,has been calibrated with the intensity of m/z 238 in the sample and m/z 239, m/z 242 in the aqueous solution of 2% nitric acid. The minimum detection limit (MDL) is 43 fg, and the lower limit of determination (LLD) is 88 fg. Among the samples analyzed,the amount of 239Pu in the open area water is larger than the MDL,while it is lower than MDL in the deep well water,and the concentrations of ()239Pu are 1.1 fg/L and 0.68 fg/L in the regional lake and river,respectively.
【Key words】 239Pu; water; polyatomic ion; inductively coupled plasma mass spectrometry; anion (exchange);
- 【文献出处】 核化学与放射化学 ,Journal of Nuclear and Radiochemistry , 编辑部邮箱 ,2004年01期
- 【分类号】X837
- 【被引频次】16
- 【下载频次】258