Matrix Modification for Atomic Absorption Spectrophotometric Determination of Volatile Elements (Ⅱ). Determination of Trace Germanium by Electrothermal Atomization

휘발성 원소들의 원자흡수 분광분석을 위한 매트릭스 개선에 관한 연구(제2보). 전열 원자화에 의한 흔적량 게르마늄의 정량

  • 최호성 (고려대학교 자연과학대학 화학과) ;
  • 최종문 (고려대학교 자연과학대학 화학과) ;
  • 김영상 (고려대학교 자연과학대학 화학과)
  • Published : 19960200

Abstract

A matrix modification was studied for the determination of trace germanium in mineral waters by electrothermal atomic absorption spectrophotometry (ET-AAS). For this, the type and quantity of modifier as well as the use of auxiliary modifier were investigated to realize the efficient modification. Germanium suffers from low sensitivity and poor reproducibility in ET-AAS determination because of the premature loss of germanium via volatile germanium monoxide formation when heated in the presence of carbon. Therefore, the addition of a matrix modifier is necessary to stablize the germanium, thermally and chemically. By the addition of palladium (10 ${\mu}g/mL)$ as a single modifier to the sample containing 500 ng/mL germanium, the charring temperature could be raised from 800 to $1000^{\circ}C$, and its absorbance was also increased, but the atomization temperature was not raised. In this case, the absorbance of germanium was not changed in the range of 10∼70 ${\mu}g/mL$ of palladium added. On the other hand, it was considered that the use of a mixed modifier could modifiy the matrix more effectively than with a single modifier. The best results were obtained by using 1% ammonium hydroxide as an auxiliary modifier together with 10 ${\mu}g/mL$ palladium. The charring temperature could be raised from 800 to $1100^{\circ}C$, without any change of the atomization temperature. With above optimum conditions, the trace amount of germanium in several mineral waters were determined by a calibration curve method, and good recoveries of more than 95% were also obtained in the samples in which a given amount of germanium was spiked. The detection limit of this method was about 6.9 ng/mL.

Keywords

References

  1. Anal. Chim. Acta. v.67 Jhonson, D.J.;West, T.S.;Dagnall, R.M.
  2. J. Anal. At. Spect. v.5 Hermann, O.H.;Chonghua, J.
  3. 대한화학회지 v.39 no.3 최종문;최호성;김영상
  4. Spectrochim. Acta. v.41B Sclemmer, G.;Welz, B.
  5. Comprehensive Organometallic Chemistry(Vol. 2) Wilkinson, S.G.;Stone, F.G.;Abel, E.W.
  6. 화학약품대사전 문성명
  7. Anal. Chem. v.26 Frederick, W.J.;White, J.A.;Biber, H.E.
  8. Analyst v.76 Cluley, H.J.
  9. Sovent Extraction in Flame Spectroscopic Analysis Cresser, M.S.
  10. A Handbook of Inductively Coupled Plasma Spectrometry Thompson, M.;Walsh, J.N.
  11. Spectrochim. Acta. v.45B Weikang, X.;Jigui, L.
  12. Colormetric Determination of elements Charlot, G.
  13. Spectrochim. Acta. v.22 Amos, M.D.;Willis, J.B.
  14. Anal. Chim. Acta. v.142 Joy, M.;Rosamilia, J.M.
  15. Spectrochim Acta v.42B Kolb, A.;Muller-Vogt, G.;Wendle, W.;Stoebel, W.
  16. Anal. Chim. Acta v.107 Mino, Y.;Shimomura, S.;Ota, N.
  17. Talanta v.34 Sohrin, Y.;Isshiki, K.;Kuwamoto, T.
  18. At. Absorp. Newsl. v.6 Manning, D.C.
  19. Spectrochim. Acta. v.42B Ni, Z.M.;Shan, X.Q.
  20. Analyst v.110 Dittrich, K.;Mandry, R.;Mothes, W.;Judelevic, J.G.
  21. Talanta v.16 Kirkbright, G.F.;Sargent, M.;West, T.S.