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Pressurized Acid Vapor Decomposition of Highly Pure Silica and Determination of Impurities by One-drop Atomic Spectrometry

高纯二氧化硅加压酸气分解及一滴原子光谱法测定杂质

基本信息

批准号：
62470033
负责人：
KOJIMA Isao
金额：
$ 3.39万
依托单位：
Nagoya Institute of Technology
依托单位国家：
日本
项目类别：
Grant-in-Aid for General Scientific Research (B)
财政年份：
1987
资助国家：
日本
起止时间：
1987 至 1988
项目状态：
已结题

项目摘要

In a sealed double Teflon vessel with stainelss steel jacket, the purification of acids and the determination of highly pure silica with these purified acid vapors were simultaneously carried out at an elevated temperature. A significant decrease in the metal blank level even from the artificially contaminated acids containing 1 mg of each metal was obtained. Trace metal impurities (Na, Ca, Mg, Cu, Fe, Mm and Ti) in natural silica, "Specpure" silica from Johnson Matthey and highly pure and synthetic silica were well determined by "One-drop" flame atomic absorption and inductively coupled plasma atomic emission spectrometries, without any other concentration step before determination.Metals extracted as their complexes into organic solvents (CC1_4, CHC1_3, CH_2C1_2 and MIBK) were determined by "One-drop" flame atomic absorption spectrometry with injection volume of 30-40 ul and without deuterium background correction. Direct injection of organic extracts of more than 50 ul into an airacetylen flame gives an interesting signal profile, which depends on the kind of metals of interest (Cu(I,II), Cd, Co, Fe(II,III), Ni and Zn). On the other hand, only normal signal profiles are obtained irrespective of metals with a nitrous oxide-acetylene flame. This interesting signal profile of a metal seems to be related to the dissociation energy of the corresponding metal oxide. The method was successfully applied to the determination of copper in certified reference material from the National Institute for Environmental Studies (NIES-CRM, No. 9, Sargasso) and the results agreed well with the certified value.

在不锈钢夹套的双层聚四氟乙烯密封容器中，在高温下同时进行酸的净化和高纯二氧化硅的测定。甚至从含有1 mg每种金属的人工污染酸中获得金属空白水平的显著降低。痕量金属杂质本文采用“一滴法”火焰原子吸收光谱法和电感耦合等离子体原子发射光谱法测定了天然二氧化硅、约翰逊万泰公司的“Specpure”二氧化硅、高纯二氧化硅和合成二氧化硅中的Na、Ca、Mg、Cu、Fe、Mm和Ti等金属元素，测定前无需任何富集步骤。采用“一滴”火焰原子吸收光谱法，进样量为30-40 μ l，无需氘背景校正。将大于50 μ l的有机提取物直接注入空气乙炔火焰中给出了令人感兴趣的信号分布，其取决于感兴趣的金属（Cu（I，II）、Cd、Co、Fe（II，III）、Ni和Zn）的种类。在另一方面，只有正常的信号配置文件得到与一氧化二氮-乙炔火焰的金属无关。金属的这种有趣的信号分布似乎与相应金属氧化物的离解能有关。该方法用于国家环境研究所标准物质（NIES-CRM，No. 9，Sargasso）中铜的测定，结果与标准值相符。