1998 Fiscal Year Final Research Report Summary
Development and evaluation of substoichiometric isotope dilution mass spectrometry as definitive method
| Project/Area Number |
09640714
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| Research Category |
Grant-in-Aid for Scientific Research (C)
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| Allocation Type | Single-year Grants |
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| Section | 一般 |
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| Research Field |
分離・精製・検出法
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| Research Institution | IBARAKI UNIVERSITY |
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Principal Investigator |
IMURA Hisanori IBARAKI Univ.Fuc.of Science.Prof., 理学部, 教授 (60142923)
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| Co-Investigator(Kenkyū-buntansha) |
OHASHI Kousaburo IBARAKI Univ.Fuc.of Science, Prof., 理学部, 教授 (60007763)
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| Project Period (FY) |
1997 – 1998
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| Keywords | Substoichiometry / Substoichiometric separation / Substoichiometric isotope dilution mass spectrometry / MIP-MS / ICP-MS / Iron / Copper / Environmental reference materials |
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| Research Abstract |
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.
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