電位差滴定法およびガスクロマトグラフ法によるベンゾトリアゾールおよびメチルベンゾトリアゾールの簡易迅速分析法

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タイトル別名
  • A simple and rapid method for determination of benzotriazol and methylbenzotriazols by potentiometry and gas chromatography
  • デンイサ テキテイホウ オヨビ ガスクロマトグラフホウ ニ ヨル ベンゾトリアゾール オヨビ メチルベンゾトリアゾール ノ カンイ ジンソク ブンセキホウ
  • Analysis of organic nitrogen compounds. XV
  • 有機窒素化合物の分析法(第15報)

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説明

The method for routine analysis of benzotriazol (BT) and methylbenzotriazol (MBT) were established by using potentiometry and gas chromatography.<BR>When the sample was dissolved in 1.5% aqueous solution of sodium bicarbonate, the most definitive end point in the potentiometric titration with silver nitrate solution was obtained (Fig. 1 and 2).<BR>If the sample contains chloride, the interference with chloride can be avoided by addition of an excess of EDTA (Fig. 3).<BR>As Table I shows, 2 to 30 mg of BT or MBT was determined successfully by this method.<BR>Each content in mixtures of BT and MBT is determined by the potentiometric titration combined with extraction procedure. For example, 100 mg of the mixtures was dissolved in 10 ml of a mixed solvent (chlorobenzene : carbon tetrachloride =1 : 1, v/v), and 10 ml of water was added to it. After the mixture had been shaked for 30 min at a room temperature (20°C), an aliquot of aqueous phase was transferred to a beaker, and 100 ml of 1.5% aqueous solution of sodium bicarbonate was added to it. The solution was titrated by the potentiometric method, in which a silver and glass electrode were employed as an indicator and reference electrode, respectively.<BR>As Fig. 5 and 6 show, the extractability reveals a good linear relation with the composition of sample, therefore, the calibration line can be applied to determine the mixtures of BT, 4-MBT and 5-MBT.<BR>In case of the mixture, gas chromatography was also useful in the microanalysis. The optimum conditions were as follows-glass column; 1 m×3 mφ, supporter; Chromosorb W(60 to 80 mesh) coated with 1.5% of neopentyl glycol sepagate, column temperature; 180°C, injection temperature; 200°C, carrier gas; nitrogen (30 ml/min), FID gas presser; hydrogen (0.5 kg/cm2) and air(1.0 kg/cm2), sensitivity and range; 103×128, sample; 1 to 5 μl of acetone solution.<BR>A chromatogram and a calibration line obtained with the above conditions were shown in Fig. 7 and 8.<BR>These methods were simple and rapid, and successfully applied to determine BT, MBT and the mixture in various commercial products(Table II, III and IV).

収録刊行物

  • 分析化学

    分析化学 22 (8), 1036-1041, 1973

    公益社団法人 日本分析化学会

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