Determination of Bi Impurity in Lead Stock Standard Solutions by Hydride-generation Inductively Coupled Plasma Mass Spectrometry

  • Park, Chang J. (Korea Research Institute of Stadards and Science)
  • Published : 2004.02.20


Total impurity analysis of a primary standard solution is one of the essential procedures to determine an accurate concentration of the standard solution by the gravimetry. Bi impurity is determined in Pb standard solutions by inductively coupled plasma mass spectrometry (ICP-MS). The direct nebulization of the Pb standard solution produces a significant amount of the Pb matrix-induced molecular ions which give rise to a serious spectral interference to the Bi determination. In order to avoid the spectral interference from the interferent $^{208}PbH^+$, the hydride generation method is employed for the matrix separation. The Bi hydride vapor is generated by reaction of the sample solution with 1% sodium borohydride solution. The vapor is then directed by argon carrier gas into the ICP after separation from the mixture solution in a liquid-gas separator made of a polytetrafluoroethylene membrane tube. The presence of 1000 ${\mu}$g/mL Pb matrix caused reduction of the bismuthine generation efficiency by about 40%. The standard addition method is used to overcome the chemical interference from the Pb matrix. Optimum conditions are investigated for the hydride-generation ICPMS. The detection limit of this method is 0.5 pg/mL for the sample solutions containing 1000 ${\mu}$g/mL Pb matrix.


  1. Watters, R. L. The First Draft on the Isotope Dilution MassSpectrometry Protocol for ICP-MS; National Institute of Standardsand Technology: Gaithersburg, MD, USA, April 1995.
  2. Sharp, B. L. J. Anal. At. Spectrom. 1988, 3, 613.
  3. Douglas, D. J.; Kerr, L. J. Anal. At. Spectrom. 1988, 3, 749.
  4. Beauchemin, D.; McLaren, J. W.; Berman, S. S. SpectrochimicaActa 1987, 42B, 467.
  5. Richner, P. J. Anal. At. Spectrom. 1993, 8, 927.
  6. Park, C. J. Bull. Korean Chem. Soc. 2002, 23, 1541.
  7. Vanhoe, H.; Goosens, J.; Moens, L.; Dams, R. J. Anal. At. Spectrom.1994, 9, 177.
  8. Zhou, N.; Frech, W.; Lundberg, E. Anal. Chim. Acta 1983, 153,23.
  9. Cadore, S.; Baccan, N. J. Anal. At. Spectrom. 1997, 12, 637.
  10. Hall, G. E. M.; Pelchat, J. C. J. Anal. At. Spectrom. 1997, 12, 97.
  11. Powell, M. J.; Boomer, D. W.; McVicars, R. J. Anal. Chem. 1986,58, 2864.