1,2-エピチオアルカンの同定と定量

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For identification and determination of 1, 2-epithioalkanes (EPA), total and thiirane sulfur of them were determined. Investigations by GLC, TLC, UV, IR, NMR and GC-MS of EPA were also carried out for the same purpose. The samples employed were 1, 2-epithio derivatives of octane, decane, dodecane, tetradecane, hexadecane and octadecane. The results of GLC with Silicone DC 430 columns were in fair agreement with the data of total sulful content. 1, 2-Epithiohexadecane and 1, 2-epithiooctadecane, however, were degraded during GLC. For such compounds, TLC with silica gel G and petroleum ether was preferable. Determination methed of thiirane sulfur with iodine-acetic acid solution gave unsatisfactory results. Molecular extinction coefficients of EPA were 40.143.2 at λmax 261262 nm in heptane solution. The IR spectra of EPA and 10, 11-epithioundecanoic acid showed four characteristic bands near 681, 646, 622, and 604 cm-1. By the application of these bands, the concentration of EPA in CCl4 solution was able to be determined, even if small amount of α-olefins or 1-thiols was present. The peaks of the protons of methylene and methyne of thiirane ring appeared at 7.75 τ (quartet) and 7.25τ (quintet) in CCl4 solution, respectively. In the mass spectrum of 1, 2-epithiodecane, parent peak did not exist, but M-32 peak due to elimination of sulfur from the compound appeared Base peak was a peak at m/e 41 due to C3H5+ .From the above results, following methods are suitable for the identification and determination of EPA : Combination of GLC and IR for the identification ; combination of GLC and total sulfur content for the determination. For the compounds degraded during GLC, following methods are recomended : Combination of TLC and IR for the identification ; combination of IR and total sulfur content for the determination.
日本油化学会の論文

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須原康夫
東京工業試験所

1,2-エピチオアルカンの同定と定量

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