| Project/Area Number |
10640586
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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 | Kanazawa University |
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Principal Investigator |
HONJO Takaharu Kanazawa University, Faculty of Science, Department of Chemistry, Professor, 理学部, 教授 (90019498)
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| Project Period (FY) |
1998 – 1999
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| Project Status |
Completed (Fiscal Year 1999)
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| Budget Amount *help |
¥3,200,000 (Direct Cost: ¥3,200,000)
Fiscal Year 1999: ¥1,500,000 (Direct Cost: ¥1,500,000)
Fiscal Year 1998: ¥1,700,000 (Direct Cost: ¥1,700,000)
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| Keywords | Crown ether / Precious metal ion / Solvent extraction / Separation analysis / 分離分析 |
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| Research Abstract |
The effect of various factors (solvent, reagent concentration, crown ether, hydrochloric acid, stripping reagent, shaking time etc.) on the extraction and back-extraction of palladium (II) in hydrochloric acid (1〜10 mol/L) and thiocyanate media with dicyclohexyl-18-crown-6 (DC18C6) in organic solvent has been investigated in detail.
On the basis of the results, the recommended procedure is proposed as follows : an aliquot(10 mL) of a sample solution containing palladium(10 μ g/mL) and potassium thiocyanate (0.05 mol/L) in 1 mol/L hydrochloric acid was placed into a 30 mL glass-stoppered centrifuge tube. A 10 mL of chloroform solution containing 0.05 mol/L DC18C6 was added to the centrifuge tube, and the mixtures were shaken on a shaking machine for 5 min. The two phases were separated by centrifugation at 2000 rpm for 5 min, and then taken by pipetting into another tube. The organic phase (10 mL) containing the extracted palladium was shaken with 10 mL of 0.1 M ammonia buffer (0.1 mol/L NH4Cl: 0.1 mol/L NH3 = 1:1) solution for 5 min. The amount of palladium stripped from the organic phase was determined by flame AAS. Palladium in hydrochloric acid and thiocyanate media has been extracted quantitatively in chloroform with DC18C6 as an ion-association species of [K・DC18CィイD26ィエD2ィイD1+ィエD1]ィイD22ィエD2[Pd(SCN)ィイD24ィエD2ィイD12-ィエD1]. The content of palladium in chloroplatinic acid of guaranteed reagent grade after its separation by DC18C6 extraction was found to be 31.66 μ g/g.
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