Development and evaluation of substoichiometric isotope dilution mass spectrometry as definitive method

亚化学计量同位素稀释质谱作为确定方法的开发和评估

• 批准号: 09640714
• 负责人: IMURA Hisanori
• 金额: $ 1.98万
• 依托单位: IBARAKI UNIVERSITY
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (C)
• 财政年份: 1997
• 资助国家: 日本
• 起止时间: 1997 至 1998
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-09640714/
• 关键词: Substoichiometry; Substoichiometric separation; Substoichiometric isotope dilution mass spectrometry; MIP-MS; ICP-MS; Iron; Copper; Environmental reference materials; 不足当量同位体希釈分析

A new analytical method, substoichiometric isotope dilution mass spectrometry (SIDMS), was proposed by combining isotope dilution mass spectrometry (IDMS) with substoichiometry. Solvent extraction and ion exchange were studied for the substoichiometric separation of trace iron(III) and copper(II), and a microwave induced plasma mass spectrometer (MIP-MS) and ICP-MS were used for the isotope measurement. By applying these methods to some environmental reference materials, the following were evaluated : accuracy, precision and practicability.1) The substoichiometric extraction of iron(III) was examined using synergistic effect based on hydrogen bond. Jron(III) in 0.1 mug levels was extracted with a substoichiometric amount of 4-isopropyltropolone in the presence of an excess of 3,5- dichlorophenol as a synergist.2) Optimum conditions in the MIP-MS measurement were examined for iron in organic solutions. The SIDMS for iron was applied to a seaweed reference material (NIES No.9), and it was confirmed that the determined value of iron well agreed with the certified value.3) The substoichiometric ion exchange separation was examined for trace iron(III). The anionic iron(III) complex formed with a substoichiometric amount of cyclohexane-1,2-diaminetetraacetate was separated from unreacting iron(III) by the cation exchange. The determination of iron in l0ng levels by SIDMS can be expected.4) Copper(II) was substoichiometrically extracted with zinc(II) diethyldithiocarbamate in carbon tetrachloride, and then the extracted copper(II) was back-extracted with a substoichiometric amount of palladium (II) into the aqueous phase. The determination of copper in 10ng levels can be expected.5) The SIDMS for copper was applied to a marine sediment reference material (NIES No.12). The content determined was close to the reference value reported by NIES.

将同位素稀释质谱法（IDMS）与亚化学计量法相结合，提出了一种新的分析方法-亚化学计量同位素稀释质谱法（SIDMS）。研究了溶剂萃取和离子交换法分离痕量铁（III）和铜（II）的方法，并采用微波诱导等离子体质谱（MIP-MS）和电感耦合等离子体质谱（ICP-MS）进行了同位素测定。将这些方法应用于环境标准物质，评价了方法的准确度、精密度和实用性。1）利用氢键协同效应研究了铁（III）的亚化学计量萃取。在过量的3，5-二氯苯酚作为增效剂的存在下，用亚化学计量量的4-异丙基环庚三烯酚酮萃取0.1 μ g水平的Jron（III）。2）对有机溶液中铁的MIP-MS测量的最佳条件进行了检查。将该方法应用于海藻标准物质（NIES No.9），测定结果与标准值吻合良好。3）采用亚化学计量比离子交换法测定微量铁（III）。与亚化学计量量的环己烷-1，2-二胺四乙酸盐形成的阴离子铁（III）络合物通过阳离子交换与未反应的铁（III）分离。用二乙基二硫代氨基甲酸锌（II）在四氯化碳中亚化学计量萃取铜（II），然后用亚化学计量的钯（II）反萃取铜（II）到水相中。5）将SIDMS用于海洋沉积物标准物质（NIES No.12）中铜的测定。测定的含量接近NIES报告的参考值。

项目成果

H.Imura: "Synergistic Extraction of Gallium (III) and Indium (III) with 2, 4-Pentaredrone and 3, 5-Dichlorophenol on the Basis of Outer-sphere Complexation" Anal.Sci.14. 1093-1098 (1998)

H.Imura：“基于外球络合，用 2, 4-Pentaredrone 和 3, 5-二氯苯酚协同萃取镓 (III) 和铟 (III)”Anal.Sci.14。

H.Imura: "Substoichiometric Isotope Drlution Mass Spectrometry As A New Analytical Method" J.Radioanal.Nucl.Chem.220. 191-193 (1997)

H.Imura：“亚化学计量同位素稀释质谱法作为一种新的分析方法”J.Radioanal.Nucl.Chem.220。

H.Imura: "Isotope Dilution Analysis and Isotope Dilution Mass Spectrometry for Iron Based on Substoithiametry" Proceedings of International Trace Analysis Symposium. 9-10 (1998)

H.Imura：“基于亚硫测量的铁的同位素稀释分析和同位素稀释质谱”国际痕量分析研讨会论文集。

H.Imura: "Substoichiometric Separation and Isotope Dilution Mass Spectrometry of Iron (III) Based on the Synergistic Extraction with 4-Isopropyltropolone and 3,5-Dichlorophenol" Anal.Sci.13 (supplement). 11-12 (1997)

H.Imura：“基于 4-异丙基托酚酮和 3,5-二氯苯酚协同萃取的铁 (III) 亚化学计量分离和同位素稀释质谱”Anal.Sci.13（补充）。

H.Imura: "Synergistic Extraction of Gallium (III) and Indium (III) with 2,4-Pentanedione and 3,5-Dichlorophenol on the basis of Outer-Sphere Complexation" Anal.Sci.14. 1093-1098 (1998)

H.Imura：“基于外层络合，用 2,4-戊二酮和 3,5-二氯苯酚协同萃取镓 (III) 和铟 (III)”Anal.Sci.14。