The spatial distribution and photometric and analytical accuracy of Sn determined by graphite furnace atomic absorption spectrometry in the presence of sulfates and palladium


Ozcan M., Akman S., Schuetz M., Murphy J., Harnly J.

JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY, cilt.17, sa.5, ss.515-523, 2002 (SCI İndekslerine Giren Dergi) identifier identifier

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 17 Konu: 5
  • Basım Tarihi: 2002
  • Doi Numarası: 10.1039/b200613h
  • Dergi Adı: JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY
  • Sayfa Sayıları: ss.515-523

Özet

The vertical spatial distribution of Sn in the graphite furnace was determined in the presence of 0.5% HCl (standards) and 10 mug of KCl, K2SO4, and NiSO4, with and without 5 mug of Pd, using a spectrometer capable of measuring spatially resolved absorbance. A normal gradient (decreasing concentration with increasing height in the furnace) was observed for Sn in HCl and KCl. This gradient was dramatically reversed in the presence of K2SO4 (at all pyrolysis temperatures) and NiSO4 (at pyrolysis temperatures below 900 degreesC) and was accompanied by poor analytical recoveries. Accurate analytical recoveries and a normal gradient were obtained for NiSO4 when a pyrolysis temperature of 900 degreesC was used. Pd yielded normal gradients statistically different (steeper) than those obtained with Sn Standards in HCl. The gradient for Sn in the presence of Pd was not affected by 10 mug of KCl, K2SO4, and NiSO4. Accurate analytical recoveries were obtained for Sn in Pd in all the matrices tested in this study and at all pyrolysis temperatures. The change in the Sn gradient induced by KCl, K2SO4, and NiSO4 resulted in photometric errors that are problematic for conventional, line-source AAS. Selection of the height of the viewing region within the furnace can exacerbate or improve the analytical recoveries. The constant Sn gradient established by Pd removed photometric error as an error source in the determination of Sn.