【作者】 王莹莹；

【导师】 张丽娟；

【作者基本信息】 北京化工大学 ， 分析化学， 2008， 硕士

【摘要】 锌元素和硒元素是人和动物生命活动中必需的微量营养元素。它们广泛分布于机体的各个部分,对生长发育和组织修复过程,增强机体免疫功能以及提高智商等有着重要的作用。研究锌元素和硒元素的准确测量有着至关重要的意义本论文基于电感耦合等离子体质谱仪准确测量的优势,展开对锌元素和硒元素适用于复杂基体的同位素稀释质谱法的分离技术研究。主要成果有:(1)阴离子交换分离法分离锌元素。对分离效率、树脂柱高度等分离条件进行了讨论,回收率在96%以上。并应用于同位素稀释质谱法测量大豆粉、人血清、牛肝样品中的锌,结果准确可靠。阴离子交换分离法分离锌元素高效、准确、方便;(2)巯基棉分离法分离硒同位素。讨论了分离效率、巯基棉交换容量等分离条件对回收率的影响,回收率在92%以上。成功分离不同丰度的同位素标准溶液及复杂样品中添加硒同位素,未引起明显的同位素分馏。此方法应用于同位素稀释质谱法测量人血清、牛肝样品中的硒,结果准确,在标准值不确定度范围内。此方法也可用于复杂基体中硒同位素的分离。本论文还涉及了锌同位素基准物质的制备研究,其中应用了锌的分离方法、浮力校正等。将两种高纯度丰度的浓缩同位素按比例定量混合,配制混合同位素基准溶液,用混合后得到的基准对质谱仪的系统偏差进行校正,用来修正样品的测量结果。这是国际上公认的获得准确同位素丰度值的一种方法。更多还原

【Abstract】 Zinc and selenium are necessary nutrient trace element in the life activity of human and animals which are extensively distributing everywhere in the body. They exert significantly influence on growth and develop, body repairing, body immunity and intelligence quotient.In present dissertation, experimental studies of separate techniques of zinc and selenium for matrix analysis with isotope dilution mass spectrometry (IDMS) were carried out. The main achievements obtained in this research are: (1) The separation of zinc with anion exchange resin. Separation conditions such as separation efficiency and column height were discussed. The recovery of zinc is above 96%. Combined with IDMS, this method was applied in determination zinc in soybean, human serum and bovine liver. The results are accurate and credible. (2) The separation of selenium isotope with sulphydryl cotton. Separate conditions such as efficiency and exchange capacity were discussed. The recovery of selenium is above 92%. Standard solution of different isotopic abundance were successfully separated. Combined with IDMS, this method was applied in determination selenium in human serum and bovine liver. The result is in the range of uncertainty of standard value. These separate techniques can also be applicated in separation of selenium isotope in compound matrix.This dissertation also refered to the research of isotopic standard, And the separate technique of zinc was applied and buoyancy correction was considered. Two highly purified and high concentrated isotope were blended to prepare isotope standard samples by gravimetry using exact balance. According to measurement of isotope standards by mass spectrometry, the correction factor of system error of mass spectrometry can be confirmed. The method is accepted by IUPAC to obtain accurate isotopic abundance of samples.更多还原