Chromotropic Acid를 착화제로 이용한 이온쌍 액체 크로마토그래피에 의한 붕소의 분리와 정량

Determination of Boron by Ion Pair Liquid Chromatography with Chromotropic Acid

  • 윤영자 (숭실대학교 이과대학 화학과) ;
  • 유구용 (삼육대학교 이과대학 화학과)
  • 발행 : 19950400

초록

chromotropic acid (1,8-Dihydroxynaphthalene-3,6-disulfonic acid)를 착화제로 이용한 붕소에 대한 분리 정량을 이온쌍 액체 크로마토그래피로 연구하였다. 이동상$(MeOH\; 61{\%},\;H_2O\;39{\%}$, 인산완충용액 pH=8.5)에 tetrabutylammonium bromide를 첨가하므로서 붕소-chromotropic acid 착물과 chromotropic acid를 poly(styrene-devinylbenzene) 역상컬럼(PRP-1, 15 $cm{\times}4.6$ mm i.d.) 상에서 분리할 수 있었으며, 또한 시료 용액중에 0.1 M의 tetrabutylammonium bromide를 첨가하므로 붕소와 chromotropic acid간의 착물형성을 촉진시켜 감도를 높일수가 있었다. 0.5~1000 ${\mu}g/L$ 농도범위에서 좋은 직선성을 나타내었고 검출 한계는 0.5 ${\mu}g/L$ (S/N=2)이었다. 제안된 방법으로 시판용 시약, $Na_2SO_4,\; NaOH,\; KCl$에 있는 미량의 붕소를 정량하였다.

The separation and determination of boron with chromotropic acid (1,8-Dihydroxynaphthalene-3,6-disulfonic acid) as a complex agent has been studied using ion pair liquid chromatography. The use of tetrabutylammonium bromide added as an ion pair reagent to mobile phase (MeOH 61%, phosphate buffer 39% pH=8.5) allowed good separation of boron-chromotrophic acid complex anion and chromotrophic acid on poly(styrene-divinylbenzene) based reversed phase column (PRP-1, 15 $cm{\times}4.6$ mm i.d.). The complex formation between boric acid and chromotrophic acid was enhanced in the presence of 0.1 M tetrabutylammonium bromide, resulting in high sensitivity. The linear calibration was achieved over the boron concentration range of 0.5∼1000 ${\mu}g/L.$ The detection limit was 0.5 ${\mu}g/L$ (S/N=2). The proposed method was applied to the determination of boron in commercially available chemicals, $Na_2SO_4$, NaOH, KCl.

키워드

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