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Journal of the Korean Chemical Society (JKCS)

ISSN 1017-2548(Print)
ISSN 2234-8530(Online)
Volume 38, Number 5
JKCSEZ 38(5)
October 20, 1994 

Spectrophotometric Determination of Trace Selenium in Aqueous Solutions by Catalytic Reaction

촉매반응을 이용한 수용액중 흔적량 셀렌의 분광광도법 정량
Seung-Hwa Lee, Jong-Moon Choi, Hee-Seon Choi, Young-Sang Kim

이승화, 최종문, 최희선, 김영상
셀렌이 촉매작용을 하는 반응을 이용한 수용액중 흔적량 셀렌의 분광광도법 정량에 관하여 검토하였다. 즉, 산성의 수용액 매질에서 셀렌에 의한 페닐히드라진의 촉매반응은 H-acid(8-아미노-1-나프톨-3,6-이슬폰산의 이나트륨염)과 반응하여 붉은 색의 아조 염료로 변하는 벤젠디아조뮴이온을 생성한다. 이 반응에 대해, 시약들의 가하는 양과 용액의 pH등과 같은 실험조건들을 최적화시켰다. 시료용액 15ml를 0.1 M EDTA용액으로 처리하여 철 등을 제거한 다음에 0.06 M 페닐히드라진 염산 1 ml, 0.02 M H-acid 1 ml, 및 0.3 M-KClO4 3 ml를 용액에 순서대로 가하였다. 염산으로 용액의 pH를 1.4로 조정하였다. 끓는 물중탕에서 30분간 가열한 다음, 식혀서 탈염수로 25.00ml되게 묽혔다. 흡광도 측정을 위한 바탕용액은 탈염수로 만들었다. 527nm에서 흡광도를 측정하였다. 위의 실험과정으로 표준검정곡선법에 의해 수도물, 강물, 및 저수지물 등의 물시료중 흔적량 셀렌을 정량하고, 시료들에 가해진 일정량의 셀렌을 정량하여 회수율을 구하였다. 이렇게 얻은 104 내지 111%의 회수율로부터 이 방법이 자연수중 ng/ml수준의 셀렌 분석에 정량적으로 응용될수 있음을 알 수 있었다.

The spectrophotometric determination of trace selenium(Ⅳ) using its catalytic reaction has been studied in aqueous solutions. The catalytic reaction of phenylhydrazine hydrochloride with selenium(Ⅳ) in an acidic aqueous medium produces benzenediazonium ion which will be converted into a red-coloured azo dye by coupling with H-acid(8-amino-1-naphtol-3,6-disulfonic acid disodium salt). For the reaction, the experimental conditions such as amounts of the reagents and pH of the sample solutions were optimized. After 15 ml of the sample solution was treated with 1 ml of 0.1 M EDTA solution to mask Fe3+, etc., 1 ml of 0.06 M phenylhydrazine hydrochloride, 1 ml of 0.02 M H-acid, and 3 ml of 0.3 M-KClO3 were added into the solution, sequentially. The solution was adjusted to pH 1.4 with HCl. After it was heated in a steam bath for 30 minutes, the solution was cooled down to a room temperature and then diluted to 25 ml with deionized distilled water. A blank solution for the absorbance measurement was prepared from the deionized water. The absorbance was measured at 527 nm. Using the above procedure, the trace amount of selenium was determined in natural waters such as tap, river and pond waters by a standard curve method and recoveries of Se spiked to samples were also obtained. From the recoveries of 104 to 111%, it could be concluded that this method was applicable to the quantitative determination of ng/ml level of selenium in natural waters.

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