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

• 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
• 来源: https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-62470033/
• 关键词: Highly pure silica; One-drop method; Atomic spectrometry; Acid vapor decomposition; Teflon decomposition; Micro scale solvent extraction; Metal complexes; 抽出試薬; テフロンボンベ; 加圧分解; 一滴法原子スペクトル分析; ICP発光分光分析; フレーム原子吸光; 炎光分析; 酸蒸気分解法; 溶媒抽出; ジチゾン錯体

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.

在带有Stainelss钢夹克的密封双双氟龙容器中，酸的纯化和用这些纯化的酸蒸气测定高度纯二氧化硅，并在温度升高的温度下同时进行。即使从含有1 mg的每种金属的人为污染的酸中，金属空白水平也显着降低。痕量金属杂质（Na，Ca，Mg，Cu，Fe，Mm和Ti）在天然二氧化硅中，来自Johnson Matthey的“ Specpure”二氧化硅以及高度纯的和合成的二氧化硅通过“单滴”火焰原子吸收和电阻性地构成等离子体的等化等上的浓度，并在没有任何其他浓度的群体中，并确定了任何其他组合物，并确定其复杂的群体。 （CC1_4，CHC1_3，CH_2C1_2和MIBK）通过“单滴”火焰原子吸收光谱测定，注射体积为30-40 ul并且没有氘背景校正。将超过50 ul的有机提取物直接注射到空气乙烯火焰中产生了有趣的信号曲线，这取决于感兴趣的金属（Cu（i，ii），CD，CO，CO，FE（II，III），Ni和Zn）。另一方面，只能获得正常信号曲线，而与一氧化二氮 - 乙炔火焰的金属无关。金属的这种有趣的信号曲线似乎与相应金属氧化物的解离能有关。该方法成功地应用于国家环境研究所（NIES-CRM，第9号，萨尔加索）的认证参考材料中的铜确定，结果与认证价值很好地一致。

项目成果

Tetsuo,Uchida: "Application of Absolute Amount Measurement in Flame Atomic Absorption Spectrometry; Extension of Linear Range of Calibration Curve (in Japanese)" Bunseki Kagaku. 37. 232-237 (1988)

Tetsuo,Uchida：“绝对量测量在火焰原子吸收光谱法中的应用；校准曲线线性范围的扩展（日语）”Bunseki Kagaku。

Isao KOJIMA: Journal of Analytical Atomic Spectrometry. 3. 583-586 (1988)

小岛功：分析原子光谱学杂志。

Isao,KOJIMA: "Determination of Copper by Flame Atomic Absorption Spectrometry Using Discrete Nebulisation of a Carbon Tetrachloride extract" Journal of Analytical Atomic Spectrometry. 3. 583-586 (1988)

Isao,KOJIMA：“使用四氯化碳提取物的离散雾化通过火焰原子吸收光谱法测定铜”分析原子光谱学杂志。

Isao KOJIMA: Journal of Analytical Atomic Spectrometry. 3. (1988)

小岛功：分析原子光谱学杂志。

Isao,KOJIMA: "Pressurized Microwave Digestion of Biological Samples for Metal Determination" Analytical Sciences. 4. 211-214 (1988)

Isao,KOJIMA：“用于金属测定的生物样品的加压微波消解”分析科学。