Nメチル-2-ピロリドン酸付加物を溶解剤とする有機金属化合物の間接定量
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Indirect etermination of organometallic compounds by means of N-methyl-2-pyrroHdone add adducts as solid dissolvent. Shigenori UTSUMI (Department of Pharmacy, Faculty of Pharmacy, Kinki University, 3-4-1, Kowakae, Higashiosaka-shi, Osaka) AT-Methyl-2-pyrrolidone (MP) reacted with inorganic acids (hydrogen chloride, hydrogen fluoride) at reaction ratio of 1 to 1 to form colorless additive compounds. Dissolving ability of the additive compounds for metals, inorganic compounds and organometallic compounds was investigated, and metals in samples were determined by direct EDTA conductimetric titration after dissolution. MP-HCl and MP-HF were prepared by passing dried gas (HCl HF) through MP at the rate of 30 ml / min. These additive compounds were stable in solid state and had relatively high melting points. Therefore the treatment of the reagents was easy to handle, and many metals and inorganic compounds were dissolved in them at comparatively low temperature without generating gases. When tin or titanium was dissolved in hydrochloric acid, it became a volatile metal chloride such as SnCl_4 or TiCl_4. But it formed a stable additive compounds with MP immediately in MP. The reaction equation was estimated as follows; Sn + 4 MP・HCl --> MP・SnCl_4 + 3 MP + 2 H_2. Silicates (BaSiO_3, CaSiO_3, CdSiO_3, MgSiO_3, MnSiO_3, PbSiO_3, NiSiOg_3, ZnSiO_3) were dissolved by the fluxes easily, too. As MP acid adducts had the both properties of organic solvents and inorganic acids, they were able to dissolve organometallic compounds. Determination of metals in organometallic compounds also could be carried out by EDTA conductimetric titration in DMSO, after dissolved the samples with the additive compounds. And organometallic compounds were indirectly determined from the measured amounts of metals. (Received Aug. 11, 1980)
- 1981-02-05
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- Nメチル-2-ピロリドン酸付加物を溶解剤とする有機金属化合物の間接定量