Determination of Lead in Steels by Hydride generation-Inductively Coupled Plama/Mass Spectrometry

수소화물 발생-유도결합플라스마 질량분석법에 의한 철강 중의 납의 정량

  • Park, Chang Joon (Division of Chemical Metrology and Material Evaluation, Korea Research Institute of Standards and Science) ;
  • Song, Sun Jin (Department of Chemistry, Yonsei University) ;
  • Lee, Dong Soo (Department of Chemistry, Yonsei University)
  • 박창준 (한국표준과학연구원 물질량표준부) ;
  • 송선진 (연세대학교 화학과) ;
  • 이동수 (연세대학교 화학과)
  • Received : 2001.09.13
  • Published : 2001.10.25

Abstract

An analytical method has been developed which determines lead in steel samples by inductively coupled plasma mass spectrometry (ICP-MS) with sample introduction by the hydride generation. The lead hydride is not stable and requires and oxidant for the oxidation into metastable Pb(IV) before reduction to $PbH_4$ with $NaBH_4$. A study was carried out to find and optimum lead hydride generation condition for a sample solution with more than $1000{\mu}g/mL$ Fe matrix. $K_2Cr_2O_7$ was found to work as an efficient oxidant when more than $10{\mu}g/mL$ Fe matrix was present. Lactic acid was used with the oxidant as a complexing agent of the metastable Pb(IV) to enhance sensitivity. Optimum concentrations of the sample acidity, oxidant and lactic acid were different depending on the matrix concentration. The isotope dilution method was employed for the quantitation of lead. The determined Pb concentrations of the NIST steel SRM 361 and 362 were in good agreement with the certified values within the uncertainty range.

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