共鳴ラマン高速液体クロマトグラフィーによる塩化ビニル樹脂中の紫外線吸収剤の定量

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タイトル別名
  • Determination of ultraviolet stabilizers in polyvinyl chloride by hplc with resonance Raman detection.
  • キョウメイ ラマン コウソク エキタイ クロマトグラフィー ニ ヨル エンカ

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抄録

Phenol-type ultraviolet (UV) stabilizers in polyvinyl chloride (PVC) were analyzed byresonance Raman detection HPLC. For selective and sensitive detection, UV stabilizers were derivatized with 4-dimethylaminoazobenzene-4'-sulfonyl chloride (DABSYL chloride). DABSYL derivatives have their absorption maximum at 460nm and show resonance Raman effect when they are irradiated with a 488.0nm line of an Ar ion laser. Analytical procedure for UV stabilizers in PVC products was as follows. UV stabilizers were separated from the PVC sample after dissolving in tetrahydrofuran. The polymer fraction was precipitated by adding methanol. After filtration, the solution was evaporated to dryness under reduced pressure. The residue was redissolved with 5ml of acetonitrile, and then ml of phenyl salicylate (Salol, internal standard) in acetonitrile was added to the solution. The solution was centrifuged to remove residual polymer. After evaporation of solvent, the residue was reacted with DABSYL chloride. A 10μl portion of the reaction mixture was injected to HPLC. DABSYL derivatives of UV stabilizers were separated by using a Shiseido Capcell Pak® C18 column (4.6i.d.×250mm) and acetonitrile/water (70/30) as an eluent at a flow rate of 1.0ml/min. Chromatograms were obtained by monitoring the resonance Raman scattering at 1136cm-1 from the flow cell which was irradiated vertically with a 488.0nm line of Ar ion laser. The calibration curve based on the relative peak height of the UV stabilizer to phenyl salicylate was linear in the concentration range of 0.1 to 1.0mg/ml for Tinuvin P (corresponding to contents of 0.04w/w% to 0.4w/w% in the PVC sample when 0.25g of the samples were taken for the analysis). The content of Tinuvin P in a PVC product determined by this method was 0.234+0.010w/w% (n=5), which was in good agreement with the theoretical value of 0.24w/w%.

収録刊行物

  • 分析化学

    分析化学 40 (5), 245-250, 1991

    公益社団法人 日本分析化学会

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